Category: alcohols-buliding-blocks

Application of 702-98-7, 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. 702-98-7, name is 2-Methyladamantan-2-ol. A new synthetic method of this compound is introduced below.

Comparative Example 1 Preparation of 2-methyl-2-adamantyl methacrylate from 2-methyl-2-adamantanol in the presence of triethyl amine 150 g (0.9 mole) of 2-methyl-2-adamantanol, 900 ml of tetrahydrofuran (THF) and 132 ml of methacrylic chloride were charged in a three neck flask, and stirred. The contents of the flask were cooled on an ice bath, and maintained at a temperature of not more than 10 C. 226 g of triethyl amine was slowly dropwise added to the resulting reaction mixture. After the mixture was reacted overnight at an ordinary temperature, iced water was portionwise added to the mixture. The reaction was further continued at -20 C. for 2 hours, and then at room temperature for one hour. An organic layer was separated from the mixture, washed with a saturated aqueous solution of sodium hydrogencarbonate and then with a saturated brine, and dried on anhydrous magnesium sulfate. The resulting product was concentrated to obtain 180 g of a raw product. Following concentration, the raw product was purified on a column of silica gel to obtain 161.4 g of a pure product (yield: 76.5%). An analysis of the thus obtained product indicated that the product was the target compound, i.e., 2-methyl-2-adamantyl methacrylate.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,702-98-7, 2-Methyladamantan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; Fujitsu Limited; US6248920; (2001); B1;,
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Related Products of 4704-94-3 ,Some common heterocyclic compound, 4704-94-3, molecular formula is C4H10O3, 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 2-hydroxymethyl-1,3-propanediol (20 g,189 mmol) in dry acetone (600 ml) freshly annealed molecularsieves (4A) and p-toluenesulfonic acid monohydrate (2 g,10.5 mmol) were added. Reaction mixture was stirred overnightat room temperature. Mixture was filtered over kieselguhr. Tothe filtrate DOWEX (D1 OH-, 7 g) was added and the mixture washeated to 40 C and stirred for 30 min. Suspension was filtered overfrit (S3) and Et3N (0.5 ml) was added to the filtrate for stabilization.Solvent was evaporated in vacuo and obtained crude material wasdried under vacuum. Crude product 24 was obtained as colourlessoil and used in the next reaction step without purification. Reactionwas monitored by TLC.

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. 4704-94-3, 2-(Hydroxymethyl)propane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; ?pa?ek, Petr; Keough, Dianne T.; Chavchich, Marina; Dra?insky, Martin; Janeba, Zlatko; Naesens, Lieve; Edstein, Michael D.; Guddat, Luke W.; Hockova, Dana; Bioorganic and Medicinal Chemistry; vol. 25; 15; (2017); p. 4008 – 4030;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2568-33-4, name is 3-Methylbutane-1,3-diol, the common compound, a new synthetic route is introduced below. category: alcohols-buliding-blocks

To a 50 mL three-necked flask equipped with a side tower packed column charged with 20 g of molecular sieve (4 A), a condenser, a thermometer and a drying tube, 0.26 g of the iron salen complex obtained in Production Example 1, 1.04 g of isoprene glycol (10 mmol),40 g (400 mmol) of methyl methacrylate and 0.08 g of phenothiazine were charged, the flask was immersed in an oil bath set at 120 C. under atmospheric stirring conditions so that the internal temperature of the flask was 100 to 105 C., The distillate fraction was fully refluxed through molecular sieves and transesterification reaction was carried out for 11 hours while returning to the reaction system. Composition analysis of the obtained reaction solution according to Test Example 1 revealed that isoprene glycol was not detected, isoprene glycol monomethacrylate was 0.1%, and isoprene glycol dimethacrylate was 99.9%. To this reaction solution, unreacted methyl methacrylate was distilled off using a rotary evaporator, 5 g of hexane was added, and the precipitated solid was suction filtered using filter paper (removal of solid matter). 5 g of 10 w / v% nitric acid aqueous solution was added to the obtained filtrate, and washing was carried out by mixing and the aqueous layer was removed by separation (washing with an acidic solution). Saturated sodium bicarbonate water was added to the obtained hexane solution to neutralize until the pH became 7. Hexane was distilled off from the hexane solution obtained by liquid separation to obtain 2.05 g of the objective isoprene glycol dimethacrylate.Composition analysis of the obtained target product according to Test Example 1 revealed that isoprene glycol was not detected, isoprene glycol monomethacrylate was 0.1%, and isoprene glycol dimethacrylate was 99.9%. The results evaluated according to Test Examples 1 to 3 are shown in Table 1.

The synthetic route of 2568-33-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KURARAY COMPANY LIMITED; TAKAHATA, YUSUKE; KAJIYASHIKI, TSUYOSHI; HOSOKI, TOMOYA; (21 pag.)JP2018/104360; (2018); A;,
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Electric Literature of 504-63-2 ,Some common heterocyclic compound, 504-63-2, molecular formula is C3H8O2, 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.

Add hexadecane bromide (1.52 g, 5 mmol) to the reaction flask.And 1,3-propanediol (1.14 g, 15 mmol),Add 5 ml of dimethyl sulfoxide and 5 ml of tetrahydrofuran to dissolve.Add sodium hydroxide (800mg, 20mmol)The reaction was carried out for 24 hours at room temperature.Dilute with 10 ml of water,Adjust the pH to neutral with 2M dilute hydrochloric acid,Extracted with ethyl acetate 3 times,Combine the organic phase,Washed with saturated brine and concentrated.Purified by silica gel column chromatography to give compound 1.0g, Yield: 66.7%.

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. 504-63-2, 1,3-Propanediol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shenzhen Tajirui Bio-pharmaceutical Co., Ltd.; Wang Yihan; Zhao Jiuyang; (46 pag.)CN109485676; (2019); A;,
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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. 517-21-5, name is Sodium 1,2-dihydroxyethane-1,2-disulfonate, molecular formula is C2H4Na2O8S2, 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. name: Sodium 1,2-dihydroxyethane-1,2-disulfonate

Glyoxal-sodium bisulfite (2.72 g, 10.2 mmol) was added to a solution of 3-amino-5-methyl-1H-pyrazole (2 g, 20.6 mmol) in water (40 mL) and was heated to 70 C. for 25 min. The mixture was then cooled down to room temperature and sodium cyanoborohydride (2.73 g, 43.4 mmol) was added and the mixture was stirred overnight. Methanol (70 mL) was added and the mixture was stirred for 1 h. Concentrated hydrochloric acid (12 N) was added until a pH<2 was obtained and the resulting mixture was stirred at room temperature overnight. The solution was then neutralized with an aqueous solution of sodium hydroxide (1M) and the solvent was evaporated. The residue was resuspended in methanol (40 mL) and stirred for 1 h. After filtration, the solvent was evaporated and the residue was purified by chromatography on a silica gel column (eluent: EtOAc, EtOAc-MeOH, 95:5, 90:10); N1,N2-bis(5-Methyl-1H-pyrazol-3-yl)ethane-1,2-diamine was obtained as a white solid.1H NMR (400 MHz, CDCl3): delta=2.21 (s, 6H), 3.35 (s, 4H), 5.35 (s, 2H).13C NMR (100 MHz, CDCl3/CD3OD 10:1): delta=11.29, 43.86, 89.75, 142.32, 155.13.MS (ESI): m/z=221 (MH+). With the rapid development of chemical substances, we look forward to future research findings about 517-21-5. Reference:
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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.558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, molecular weight is 108.5667, as common compound, the synthetic route is as follows.Recommanded Product: 558-42-9

2,2-Dimethylmorpholine hydrochloride 1-Chloro-2-methyl-2-propanol (135 ml) was added dropwise over 10 min to stirred 2-aminoethanol (400 ml) at 10° C. under nitrogen. The cooling bath was then removed and stirring was continued at room temperature for 48 h. A solution of sodium hydroxide (48.8 g) in methanol (440 ml) was added and the resulting white suspension was stirred for 10 min. The mixture was filtered through a pad of kieselguhr and the filtrate was concentrated under reduced pressure. The residual oil was distilled in vacuo to give 1-[(2-hydroxyethyl)amino]-2-methyl-2-propanol (133 g).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,558-42-9, 1-Chloro-2-methyl-2-propanol, and friends who are interested can also refer to it.

Reference:
Patent; Akzo Nobel N.V.; US5593983; (1997); A;,
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Application of 454-91-1, 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. 454-91-1, name is 1-[3-(Trifluoromethyl)phenyl]ethanol, molecular formula is C9H9F3O, 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.

0.200 g (0.6 mmol) of (3R)-4-(4-toluenesulfonyl)thiomorpholine-3-carboxylic acid, 0.190 g (1.0 mmol) of 1-methyl-1-(3-trifluoromethylphenyl)-methanol, 0.088 g (0.33 mmol) of CAS, 0.227 g (1.2 mmol) of DCC and 0.04 g (0.33 mmol) of DMAP were dissolved in 15 mL of CH2Cl2. The mixture was stirred for 24 h at room temperature. The solid was filtrated and the solvent was evaporated. The residual was dissolved in a suitable amount of ethyl acetate (20 ml) and then the mixture was filtered to remove insoluble substance. The ethyl acetate was added to 60 ml and then the liquid was washed with 10% NaHCO3 solution, saturated NaCl solution and dried over Na2SO4. After the drying agent was removed and part of ethyl acetate was evaporated, the crude product was purified by flash column chromatography (eluent: ethyl acetate_cyclohexane=1:9) to obtain the product as a oil (0.13 g).

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 454-91-1, 1-[3-(Trifluoromethyl)phenyl]ethanol.

Reference:
Patent; Li, Song; Nie, Aihua; Shen, Beifen; Wang, Lili; Pei, Wuhong; Xiao, Junhai; Yang, Songcheng; Yun, Liuhong; Liu, Hongying; Shu, Cuiling; Wang, Hongxia; Rao, Zihe; US2005/130958; (2005); 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.455-01-6, name is 2-(3-(Trifluoromethyl)phenyl)ethanol, molecular formula is C9H9F3O, molecular weight is 190.1624, as common compound, the synthetic route is as follows.SDS of cas: 455-01-6

General procedure: DIAD (0.65mL, 3.31mmol) was added dropwise to 12a or 12b (500mg, 2.21mmol), PPh3 (869mg, 3.31mmol) and appropriate alcohol [2-phenylethanol (0.27mL, 2.21mmol, 2e; or 0.17mL, 1.46mmol, 2k), 2-(3-methoxyphenyl)ethanol (0.31mL, 2.21mmol, 2f; 0.20mL, 1.46mmol, 2l), or 2-(3-trifluoromethylphenyl)ethanol (0.33mL, 2.21mmol, 2g and 2m] in THF (10mL), and the mixture was stirred for 18h. Drying, evaporation and chromatography (PE/EtOAc 20:1) gave the esters 2e-g, k-m. Spectroscopic data for these compounds are given in the Supporting information.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,455-01-6, 2-(3-(Trifluoromethyl)phenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Article; Yevglevskis, Maksims; Nathubhai, Amit; Wadda, Katty; Lee, Guat L.; Al-Rawi, Suzanne; Jiao, Tingying; Mitchell, Paul J.; James, Tony D.; Threadgill, Michael D.; Woodman, Timothy J.; Lloyd, Matthew D.; Bioorganic Chemistry; vol. 92; (2019);,
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Synthetic Route of 4654-39-1, Adding some certain compound to certain chemical reactions, such as: 4654-39-1, name is 2-(4-Bromophenyl)ethanol,molecular formula is C8H9BrO, 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 4654-39-1.

A solution of 2-(4-bromophenyl)ethanol (4.43 g, 0.0220 mol) dissolved in CH2Cl2 (50 mL) was cooled to 0C. Next, PPh3 (6.92 g, 0.0264 mol) was added, followed by NBS (4.70 g, 0.0264 mol), and vigorous effervescence in a yellow solution was observed. The mixture was allowed to stir at 0C for 60 minutes. After this time, the yellow solution was treated with saturated sodium bicarbonate solution (20 mL). The deep, dark blue organic layer was separated, and the aqueous layer was extracted with CH2Cl2 (2 × 20 mL). The organic layers were combined and then the solvent was removed under reduced pressure to yield a deep, dark blue oil. The oil was purified on a column of silica (~1.5 cm × 20 cm) using EtOAc/hexanes (1:10) as an eluent and collecting the first nearly colourless fraction. Removal of the volatiles under reduced pressure yielded a very pale orange liquid. Yield: 5.38 g (93%). 1H NMR (500 MHz, 22C, CDCl3): 7.43 (d, 2H, 2JHH = 8 Hz, Ar), 7.08 (d, 2H, 2JHH = 8 Hz, Ar), 3.53 (t, 2H, 3JHH = 7 Hz, -CH2CH2-), 3.11 (t, 2H, 3JHH = 7 Hz, -CH2CH2-).

According to the analysis of related databases, 4654-39-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Tassone, Joseph P.; Mawhinney, Robert C.; Spivak, Gregory J.; Journal of Organometallic Chemistry; vol. 776; (2015); p. 153 – 156;,
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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.2867-59-6, name is 3-Aminobutan-1-ol, molecular formula is C4H11NO, molecular weight is 89.14, as common compound, the synthetic route is as follows.Application In Synthesis of 3-Aminobutan-1-ol

in a microwave-tube, ethyl 2-[benzyloxycarbonyl(2-oxoethyi)amino]acetate (330 mg, 1 .18 mmol) was diluted in DCM (8 ml), then (+/-)-3-aminobutan-1-ol (1 16 mg, 1.24 mmol) and acetic acid (39 muIota, 673 prnol) were added to give a colorless solution. The reaction mixture was submitted to microwave heating for 1.5 h at 140 C. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography (silica gel, 0% to 50% EtOAc in heptane) to give the title compound (183 mg, 51 %) as a colorless oil. The relative stereochemistry of the product was unambiguously assigned by NOESY NMR experiments. (1085) MS (ESI, m/z): 305.2 [(M+H)+].

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2867-59-6, 3-Aminobutan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; SAVIRA PHARMACEUTICALS GMBH; EUROPEAN MOLECULAR BIOLOGY LABORATORY; LERNER, Christian; KREIS, Lukas; HILPERT, Hans; (268 pag.)WO2017/158151; (2017); A1;,
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