Tag: M.W=200-300

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 17773-10-3, name is Choline Iodide. A new synthetic method of this compound is introduced below., Safety of Choline Iodide

Preparation of Tetraalkylammonium Hydroxides; The above TAA halides were converted to the equivalent hydroxide using the anion exchange resin, Dowex 550. The general procedure is described in detail for the exchange of choline iodide to choline hydroxide. The resin (30 g) was activated using NaOH before being thoroughly washed with distilled water. To this was added [(CH3)3N(CH2CH2OH)]I (1.99 W 8 mmol) in distilled water (50 ml). This was then agitated on a mixing plate for 24 hours. The resin was removed by filtration and further washed with distilled water (4×15 ml). The filtrate and washings were reduced on a rotary evaporator to a volume of 8 ml. The filtrate was shown to contain no halide using the silver nitrate test. An aliquot of the solution (1 ml) was diluted with water (9 ml) and titrated with HCl (0.1M) to establish the hydroxide content as 1.0M.Calculated yield=0.96 g (99%) (1M solution)

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 17773-10-3, Choline Iodide.

Reference:
Patent; PILKINGTON GROUP LIMITED; US2012/263903; (2012); A1;,
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Electric Literature of 457889-46-2, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.457889-46-2, name is (4′-(Trifluoromethyl)-[1,1′-biphenyl]-4-yl)methanol, molecular formula is C14H11F3O, molecular weight is 252.2318, as common compound, the synthetic route is as follows.

To an ice cold solution of intermediate M10 (2.02g, lequiv) in anhydrous diethyl ether (20ml) protected with a CaCl2 drying tube to insulate moisture was added phosphorus tribromide (0.38ml, 0.5equiv). The mixture was stirred at room temperature for 1.5h to obtain a clear solution. TLC detection showed that the reaction was complete and then the mixture was quenched with saturated sodium bicarbonate solution. The resulting precipitate was filtered off and the filtrate was extracted with dichloromethane twice (40ml), dried over MgSO4, filtered and then evaporated in vacuo to give intermediate M11 (1.77g) as a white solid which could be used in next step without further purification.

The chemical industry reduces the impact on the environment during synthesis 457889-46-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Shanghai Institute of Materia Medica, Chinese Academy of Sciences; SHEN, Jianhua; WANG, Yiping; WANG, Kai; EP2725024; (2014); A1;,
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Related Products of 397323-70-5, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 397323-70-5, name is (2-Amino-3-bromophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 139-2 (1.10 g, 5.44 mmol, 1 eq) in DCM (15 mL) was added Mn02 (4.73 g, 54.44 mmol, 10 eq). The mixture was stirred at 25 C for 1 hr. The reaction mixture was filtered and concentrated under reduced pressure to give 139-3 (1 g, crude) as a black oil.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 397323-70-5, (2-Amino-3-bromophenyl)methanol.

Reference:
Patent; VIVACE THERAPEUTICS, INC.; KONRADI, Andrei W.; LIN, Tracy Tzu-Ling Tang; (472 pag.)WO2020/97389; (2020); A1;,
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With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.13826-35-2, name is (3-Phenoxyphenyl)methanol, molecular formula is C13H12O2, molecular weight is 200.23, as common compound, the synthetic route is as follows.Product Details of 13826-35-2

3- (2-hydroxyphenyl) propionic acid methyl (149.8 mg, 0.831 mmol), 3- phenoxybenzyl alcohol (118.2 mg, 0.590 mmol), triphenylphosphine (198.1 mg, 0.755 mmol) in toluene (5 of 5 mL) solution of , DEAD (2M solution in toluene, 374.6muL, 0.749 mmol) was added dropwise at room temperature and stirred for 3 hours at 70 C.. The solvent of the reaction mixture was evaporated, and the residue was purified by column chromatography (hexane: ethyl acetate = 15: 1) to give the title compound (200.2mg, 0.552 mmol, 94%, yellow oil)

At the same time, in my other blogs, there are other synthetic methods of this type of compound,13826-35-2, (3-Phenoxyphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; THE UNIVERSITY OF TOKYO; TOHOKU UNIVERSITY; OHWADA, TOMOHIKO; NAKAMURA, SHO; JUNG, SEJIN; OTANI, YUKO; SAYAMA, MISA; AOKI, JUNKEN; (80 pag.)JP2016/17036; (2016); A;,
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Electric Literature of 7073-69-0 ,Some common heterocyclic compound, 7073-69-0, molecular formula is C9H11BrO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

To a solution of n-BuLi (166 mL, 2.6 M, 432 mmol) in 200 mL of THF at -78 C. under argon was slowly added a solution of Compound 10d (42.2 g, 196 mmol) in 60 mL of THF at a rate that the internal temperature remained below -70 C. The mixture was stirred at -75 C. for 2 h. To the reaction mixture was then added triisopropylborate (59 mL, 255 mmol) in three portions. The mixture was allowed to warm slowly to room temperature overnight. The mixture was then cooled to 0 C., and was carefully quenched with dilute hydrochloric acid (250 mL, 2N). The mixture was then stirred at room temperature for 1 h. The pH of the mixture was checked and adjusted to acidic using additional 2N HCl if prophetic. The two layers were separated, and the aqueous layer was extracted twice with ether. The organic layers were combined, and dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to yield a pale yellow oil. The residue was then diluted with ethyl acetate (400 mL) and, washed with 1N sodium hydroxide solution (150 mL×3). The basic aqueous layers were combined and acidified with 2N HCl. The clear solution turned cloudy when the acid was added. The mixture was extracted with ether (150 mL×3). The organic layers were combined and dried with magnesium sulfate. The solution was filtered, and the filtrate was concentrated under reduced pressure to yield the title Compound 10e as a colorless oil (26.2 g, 82%) which was used without further purification in the next step. 1H NMR (400 MHz, DMSO-d6) delta (ppm): 9.00 (s,1H), 7.66 (dm,1H, J=7.3 Hz), 7.45 (dt, 1H, J=1.1, 7.7 Hz), 7.40 (dm, 1H, J=7.6 Hz), 7.31 (dt, 1H, J=1.2, 7.1 Hz), 1.44 (s, 6H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 7073-69-0, 2-(2-Bromophenyl)propan-2-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Player, Mark R.; Dax, Scott L.; Parsons, William H.; Brandt, Michael Richard; Calvo, Raul R.; Patel, Sharmila; Liu, Jian; Cheung, Wing S.; Jetter, Michele C.; Lee, Yu-Kai; Youngman, Mark A.; Pan, Wenxi; Weils, Kenneth M.; Beauchamp, Derek A.; US2007/259936; (2007); A1;,
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Application of 355-80-6, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 355-80-6, name is 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol. This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of 4-methyl-2-[(2,2,3,3,4,4,5,5-octafluoropentyl)oxy]-1,3,2-dioxaphosphinane 29.90g (0.129mol) of 2,2,3,3,4,4,5,5-octafluoro-1-pentanol and 15.65g (0.155mol) of triethylamine were dissolved in 180ml of hexane to prepare a solution, and another solution was prepared by dissolving 20.00g (0.129mol) of 2-chloro-4-methyl-1,3,2-dioxaphosphinane in 20ml of hexane. The latter solution was dropped to the former solution while the former solution was fervently agitated at -10C for 3.5 hours. During the process, a formation of a white triethylammonium hydrochloride precipitate was to be found. The reaction mixture was further agitated for 3 hours at room temperature and allowed to stand for one night. The triethylammonium hydrochloride was separated from the resulting mixture and washed with hexane. Then, hexane was removed under the atmospheric pressure, and the residues were distilled under vacuum, obtaining 32.53g of a compound which is 4-methyl-2-[(2,2,3,3,4,4,5,5-octafluoropentyl)oxy]-1,3,2-dioxaphosphinane, represented by the following Chemical Formula 1A, The yield was 72%.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 355-80-6, 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol.

Reference:
Patent; Samsung SDI Co., Ltd.; Chernyshov, Denis; Shin, Woo-Cheol; Shatunov, Pavel Alexandrovich; Tereshchenko, Alexey; Egorov, Vladimir; Khasanov, Makhmut; Jeong, Myung-Hwan; EP2746288; (2014); A1;,
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Application of 133803-81-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 133803-81-3, name is tert-Butyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate, molecular formula is C11H22O5, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

DIAD (730 muL, 3.60 mmol) was added dropwise to a stirred solution of 3-methoxy-5-nitrophenol (510 mg, 2.99 mmol), tert-butyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate (700 mg, 2.99 mmol) and triphenylphosphine (950 mg, 3.59 mmol) in THF (4 mL) at 0-5 C. The reaction was allowed to warm to rt and stirred at this temperature overnight. The reaction mixture was concentrated in vacuo. The crude product was purified by chromatography on silica gel (80 g column, 0-100% EtOAc in isohexane) to afford the sub-title compound (1.13 g) as a yellow oil, which solidified on standing. The product was used in the next without further purification. 1H NMR (400 MHz, DMSO-d6) delta: 7.34-7.32 (m, 2H), 6.98 (t, 1H), 4.21-4.19 (m, 2H), 3.85 (s, 3H), 3.76-3.74 (m, 2H), 3.60-3.56 (m, 4H), 3.52-3.50 (m, 2H), 2.40 (t, 2H), 1.38 (s, 9H).

According to the analysis of related databases, 133803-81-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Topivert Pharma Limited; Respivert Limited; BAKER, Thomas Matthew; FYFE, Matthew Colin Thor; HARBOTTLE, Gareth William; HASIMBEGOVIC, Vedran; MEGHANI, Premji; RIGBY, Aaron; SAMBROOK-SMITH, Colin; THOM, Stephen Malcolm; US2014/296208; (2014); A1;,
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Adding a certain compound to certain chemical reactions, such as: 145691-59-4, (3,5-Dibromophenyl)methanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Safety of (3,5-Dibromophenyl)methanol, blongs to alcohols-buliding-blocks compound. Safety of (3,5-Dibromophenyl)methanol

3, [5-DIBROMOBENZYL ALCOHOL] (9.8 g, 36.9 [MMOL)] is dissolved in DMF (100 ml) and, while stirring, thionyl chloride (5 [ML)] is slowly added dropwise. [AFTER30 M IN,] the reaction mixture is concentrated in vacuo and the residue is taken up in EA (150 [ML). FORWORKUP,] the organic phase is washed with ice-water (50 ml) and then with half-saturated aqueous NaCi solution (50 [ML).] The organic phase is dried over [MGS04,] filtered and concentrated in vacuo. The title compound (10.4 g) is obtained as a yellow solid. TLC [PE/EA (95: [05)], RF=] 0.69.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,145691-59-4, (3,5-Dibromophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; ALTANA PHARMA AG; WO2004/12731; (2004); A1;,
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Application of 17701-61-0, Adding some certain compound to certain chemical reactions, such as: 17701-61-0, name is Benzyl 3-hydroxy-2,2-dimethylpropanoate,molecular formula is C12H16O3, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 17701-61-0.

(a) To a solution of 4-isopropyl-6-hydroxy-2-(1-phenyl-3-trifluoromethylpyrazol-5-yl-oxymethyl)-1,2-benzisothiazol-3(2H)-one 1,1-dioxide (1 g; 2.08 mmol) in THF containing (Ph)3 P (550 mg; 2.09 mmol) and DEAD (360 mg; 2.07 mmol) was added benzyl 2,2-dimethyl-3-hydroxypropionate (440 mg;2.099 mmol) and the resulting mixture was stirred at room temperature for 15 hours. The mixture was concentrated in vacuo and the residue was purified by flash chromatography (silica gel) to afford 440 mg (32%) of 4-isopropyl-6-[2-(phenylmethyloxycarbonyl-2-methyl)propoxy]-2-(1-phenyl-3-trifluoromethylpyrazol-5-yl-oxymethyl)-1,2-benzisothiazol-3(2H)-one 1,1-dioxide (Formula I: R1 =Ph; R2 =CF3; R3 =H; R4 =CH(CH3)2; R5 =6-OCH2 C(CH3)2 CO2 CH2 Ph) as a gum.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 17701-61-0, Benzyl 3-hydroxy-2,2-dimethylpropanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sanofi; US5750550; (1998); A;,
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Adding a certain compound to certain chemical reactions, such as: 112-70-9, 1-Tridecanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Recommanded Product: 112-70-9, blongs to alcohols-buliding-blocks compound. Recommanded Product: 112-70-9

EXAMPLE 3 [00079] The following Example describes the condensation esterification of DDDA using methanesulfonic acid catalyst and the preparation of DDDA diester using a mixture of 50 mole % Telomer alcohol-L and 50 mole % Exxal 13. [00080] A 500 mL round bottom flask was charged with 69.06 g DDDA (MW 230.3, 0.3 mole), 130.41 g Telomer alcohol-L (average molecular weight?414, 0.315 mole), 62.37 g Exxal 13 tridecyl alcohol from Exxon (FW?198, 0.315 mole), 0.29 g methanesulfonic acid (MW 96.1, 0.003 mole), and 100 g mixed xylenes. The reaction flask was fitted with an 8 Vigreux column topped with a Dean-Stark trap and condenser. The reaction was heated to reflux to drive off water, which was separated in the Dean-Stark trap, xylene overflow being returned to the reaction flask. The reaction was followed by water removal and by periodic sampling and titration for acid number. [00081] After 10 and ½ hours reaction time, the acid number had decreased to 1.6 mg KOH/g, and the reaction was considered to be complete. [00082] The reaction product was brown. The reaction product was washed, at 70-80 C., with 330 g of 0.2% aqueous sodium hydroxide. Phases were inverted, with a brown aqueous phase on top and the denser ester phase on the bottom. The lower ester phase was very cloudy. After separating the caustic wash, the ester phase was washed three times with 300 mL portions of warm water. The acid number was 0.56 mg KOH/g. [00083] The crude ester was sparged with nitrogen and heated from room temperature to a temperature of 210-220 C. over a period of 90 minutes to remove xylene, water, and other low boilers. [00084] The yield was 215.72 g of a waxy tan solid having an acid number 0.75 mg KOH/g. [00085] The same basic procedure as above was used to prepare other partially fluorinated esters, listed in Table 5. In all cases, the non-fluorinated alcohol was Exxal 13, tridecyl alcohol from Exxon. Due to difficulty obtaining reliable F elemental analysis, ester end groups were also analyzed by 1H NMR. The chemical shift region between 3.5 and 4.5 ppm downfield of tetramethylsilane reveals the CH2 protons attached to the ester oxygen. In the case of Rf, these CH2 protons are cleanly separated and downfield from the CH2 protons of Rh. The relative molar amounts of Rf and Rh can be calculated from the integrals of these two groups. Where elemental analysis and NMR disagree, the NMR method is believed to be more reliable. Table 5. Partially fluorinated esters prepared by condensation esterification using methanesulfonic acid catalyst[TABLE-US-00006] Mole fractionAcid PartiallypartiallynumberWt % FWt %Prepara- Fluorinatedfluorinated(mg(elementalF (bytionDiacidalcoholalcoholKOH/g)analysis)NMR) 9AdipicTelomer0.0250.341.922.6 alcohol-L10AdipicTelomer0.0250.292.253.2 alcohol11AzelaicTelomer0.02501.831.66 Alcohol-L12C14Telomer0.0250.271.391.28 diacidalcohol-L13CorfreeTelomer0.02501.231.39 M1alcohol-L14CorfreeTelomer0.0250.61.321.49 M1alcohol-L15DDDAPoly HEPO0.0250.14.17 alcohol16DDDATelomer0.025 alcohol17DDDATelomer0.0250.552.12.4 alcohol18DDDATelomer0.0250.131.862 alcohol19DDDATelomer0.0230.100 alcohol20DDDATelomer0.024000 alcohol21DDDATelomer0.0250.181.872.1 alcohol-L22DDDATelomer0.1250.243.019.47 alcohol-L23DDDATelomer0.050.2 4.06 alcohol-L24DDDATelomer0.0250.181.821.92 alcohol-L25DDDATelomer0.250.316.6817.3 alcohol-L26DDDATelomer0.50.75134.634.3 alcohol-L27DDDATelomer0.0250.272.363.4 ethoxylate alcohol28SebacicTelomer0.0250.21.581.63 alcohol-L29SubericTelomer0.0250.260.721.91 alcohol-L [00086] FIG. 4 shows the wear and friction performance of a low-F-content material (?2% F), sample 18 in Table 5, in 150N oil. This low-F-content material was completely soluble even at 20% by weight concentration (0.4 wt. percent F). FIG. 5 compares the anti-wear performance of this low-F material to a similar non-fluorinated diester, ditridecyl dodecanedioate (Hatcol 2907, from Hatco), showing the significant improvement in wear performance from only a very small amount of F incorporation. [00087] Anti-wear and friction reducing performance of different chain length diesters from C6 to C14 was compared. All of these non-symmetric, partially fluorinated diesters imparted some benefits, with the longer chain diacids giving the greater benefits. Therefore, the preferred number of carbon atoms in the backbone is 9 or more or the wear scar by the BOCLE test as described herein is less than about 0.75 when the additive is present at about 0.2% fluorine.

The synthetic route of 112-70-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. du Pont de Nemours and Company; US6734320; (2004); B2;,
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