Author: tianli

Application of 629-41-4, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 629-41-4 as follows.

In a 2 L three-opening bottle into the 1, 8 – octandiol (250 g, 1.712 muM), toluene (1000 ml), 48% hydrogen bromide (231 ml, 2 . 054 muM, 1.2 eq), heating to 110 C reflux 30 hours. Added 48% hydrogen bromide (84 ml, 0 . 753 muM, 0 . 44 eq), heating reflux for 20 hours, GC detection with a small amount of residues of raw materials. Cooling to the room temperature plus 500 ml petroleum ether dilution, liquid […] bromic acid, organic phase are saturated sodium bicarbonate (400 ml × 2) and saturated brine (400 ml × 2) cleaning, dried with anhydrous sodium sulfate. Turns on lathe does 8 – bromine propyl butyl-carbinol 318 g, yield 83%, direct throws down the step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,629-41-4, its application will become more common.

Reference:
Patent; Changzhou University; He Jiayi; Xia Ran; Wu Linsheng; Hu Xiwen; Jin Xinyu; Chen Ke; Li Yuan; Qiu Lin; Chen Xin; (8 pag.)CN109796336; (2019); A;,
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Related Products of 144-19-4, Adding some certain compound to certain chemical reactions, such as: 144-19-4, name is 2,2,4-Trimethyl-1,3-pentanediol,molecular formula is C8H18O2, 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 144-19-4.

238. 5g of 2, 2, 4-trimethyl-1, 3-pentanediol was placed (TMPD, 1.631 mol) in a 2-13- neck round-bottom flask. To this was added 205.7g DMC (2.283 mol, 40% excess) and 2.2g zinc stearate. The reaction flask was equipped with a thermocouple temperature probe, magnetic stirbar, and a 1″wide, 10″long vacuum-jacketed, silvered column packed with HastelloyG) B, atop which was placed a variable reflux K-head and condenser. The system was purged by bubbling nitrogen into the reaction mixture for 45 minutes prior to being heated. While under an atmosphere of nitrogen, the mixture was heated slowly to 100- 105C. After 30 minutes of heating, the boiling mixture began to reflux at an overhead temperature of 62-64C. The methanol byproduct/DMC azeotrope (typically a 70/30 wt/wt mixture of methanol/DMC) was removed at a reflux to takeoff ratio of between 3: 1 and 8: 1. After 2 hours of continuous heating, the temperature of the reaction mixture slowly began to rise, reaching 150-155C over the course of the next 15.5 hours as methanol was removed from the system. At this point, 37.9g DMC and 79.2g methanol (75.9% of total expected) had been removed from the reaction. The reaction mixture was then cooled to 60C and a vacuum was slowly introduced in order to remove unreacted DMC and additional methanol by-product. During this time, the temperature of the mixture was slowly increased. After 3 hours, the reaction mixture had been warmed to 90-95C and the system pressure had been reduced to 1.0-2. 0 mmHg. The system pressure was then further reduced to 0.5-1. 0 mmHg and the temperature of the mixture increased to 130C. Unreacted TMPD was preferentially removed from the reaction at an overhead temperature of 80-95C followed by distillation of the carbonate product 4-isopropyl-5, 5-dimethyl-1, 3-dioxan-2-one at an overhead temperature of 95-110C. Several cuts were taken during the distillation and analyzed by GC with the following results; Based on the above results (assuming actual wt. % is approximately equal to GC area %), reaction yield = 73.5%.

According to the analysis of related databases, 144-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUNTSMAN PETROCHEMICAL CORPORATION; WO2003/89424; (2003); A1;,
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Adding a certain compound to certain chemical reactions, such as: 34626-51-2, 5-Bromopentan-1-ol, 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, name: 5-Bromopentan-1-ol, blongs to alcohols-buliding-blocks compound. name: 5-Bromopentan-1-ol

Condensation of a-bromo aldehyde with 2,4-diamino-4-oxo-pyrimidine 19 is the key step in the synthesis of compounds 9-11 as outlined in Scheme 1 and Scheme 2. Commercially available alcohol 14 was coupled to the corresponding phenyl esters and oxidized to the corresponding aldehydes 17a and 17b (Scheme 1).-? Alcohol 24 was coupled to the appropriate phenyl ester to afford the aldehyde 25 (Scheme 2). The aldehydes were reacted with Br2 in dioxane to give the desired a-bromoaldehydes?2 18a, 18b (Scheme 1) and 26 (Scheme 2) and immediately reacted with 2,4-diamino-6-hydroxypyrimidine 19 to cyclize to the 5-substituted pyrrolo[2,3-d]pyrimidines 20a, 20b (Scheme 1) and 27 (Scheme 2).? Hydrolysis of the esters provided the free acids 21 a, 2 lb and 28. Subsequent peptide coupling with diethyl L-glutamate using the activating agents N-methyl morpholine and 2,4-dimethoxy-6-chlorotriazine, afforded the diesters 22a, 22b and 29. Saponification of the diesters yielded the final compounds 9-11 of this invention.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,34626-51-2, 5-Bromopentan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; DUQUESNE UNIVERSITY OF THE HOLY SPIRIT; WAYNE STATE UNIVERSITY; GANGJEE, Aleem; MATHERLY, Larry H.; (43 pag.)WO2016/22881; (2016); A1;,
Alcohol – Wikipedia,
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Synthetic Route of 5208-93-5, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 5208-93-5 as follows.

Analogously to example 11, vinylionol in DMF or NMP was reacted firstly with tBuOOH. The resulting reaction was then further reacted in accordance with the details in table 2 with a base to give the end product of the formula I (R?H). The yields are given in table 2:

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5208-93-5, its application will become more common.

Reference:
Patent; BASF SE; Ernst, Hansgeorg; Puhl, Michael; Benson, Stefan; Siegel, Wolfgang; US2013/116473; (2013); A1;,
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Synthetic Route of 15258-73-8 ,Some common heterocyclic compound, 15258-73-8, molecular formula is C7H6Cl2O, 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.

Compound 3-e (320 mg, 1.818 mmol) was obtained in an ice bath.Diisopropyl azodicarboxylate (400 mg, 2.00 mmol) was slowly added dropwise to a solution of 2-nitrophenol (250 mg, 1.818 mmol), triphenylphosphine (520 mg, 2.00 mmol) in tetrahydrofuran (5 mL). After stirring overnight at room temperature, the solvent was distilled off under reduced pressure, and the residue was purified by Prep-TLC (petroleum ether/ethyl acetate = 1:1) to give compound 3-d (0.30 g, 55%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,15258-73-8, its application will become more common.

Reference:
Patent; SHANGHAI KAIHUI TECHNOLOGY DEVELOPMENT CO;LTD; XU, ZUSHENG; Kaihui Science And Technology Development (Shanghai) Co., Ltd.; Xu Zusheng; (100 pag.)CN103304571; (2018); B;,
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Application of 5333-42-6, 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. 5333-42-6, name is 2-octyldodecan-1-ol, molecular formula is C20H42O, 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.

Example 6 Preparation of 2-octyldodecyl pentanoate To a 3-neck 1000 ml round-bottomed flask was added 2-octyl-1-dodecanol (140.0 g, 468.92 mmol, 1.0 equiv.), n-pentanoic acid (71.838 g, 703.40 mmol, 1.50 equiv.), toluene (175 ml) and p-toluenesulfonic acid monohydrate (0.8920 g, 4.689 mmol, 0.010 equiv.) at room temperature. The resulting mixture was heated at reflux with stirring in an oil bath at 134 C. under a nitrogen atmosphere for 12 hours. The water produced in the reaction was collected in a Dean-Stark trap. The cooled mixture was diluted with hexanes, washed with dilute aqueous 10% Na2CO3 solution, water, brine, dried (MgSO4), filtered, and concentrated in vacuo to afford a crude product. Excess solvent was further removed by heating the crude product with stirring in an oil bath under high vacuum for 3 hours to afford a light yellow liquid (178.0 g, 99%).

According to the analysis of related databases, 5333-42-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ExxonMobil Research and Engineering Company; Ng, Man Kit; Oumar-Mahamat, Halou; Cheng, Hong; Blain, David A.; Cooper, Kathleen K.; Carey, James T.; Douglass, Michael R.; Kanga, Percy R.; Patil, Abhimanyu O.; Bodige, Satish; Lewis, Kyle G.; Hagemeister, Mark P.; (40 pag.)US2017/183595; (2017); A1;,
Alcohol – Wikipedia,
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Related Products of 3637-61-4, 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.3637-61-4, name is Cyclopentanemethanol, molecular formula is C6H12O, molecular weight is 100.16, as common compound, the synthetic route is as follows.

cyclopentane methanol (119a) (500 mg) was dissolved in pyridine (5 mL), under ice cooling, added TsCl (1.43 g), and the reaction was stirred at room temperature for 36 hours. After concentrating the solvent under reduced pressure, the residue ethyl acetate(50 mL) was added to the organic layer saturated aqueous sodium hydrogen carbonate solution (50 mL), washed with saturated brine (50 mL), and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reducedpressure, the residue was purified by silica gel flash column chromatography (developing solvent nhexane:ethyl acetate =50: 1) to obtain a colorless cyclopentylmethyl tosylate (120a) (864 mg, 68% yield) to give an oil.

Statistics shows that 3637-61-4 is playing an increasingly important role. we look forward to future research findings about Cyclopentanemethanol.

Reference:
Patent; Nagoya City University; Miyata, Naoki; Suzuki, Takayoshi; Ota, Yosuke; Ueda, Ryuzo; Ida, Shinsuke; Rie, Masaki; (47 pag.)JP5725475; (2015); B2;,
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Related Products of 675580-49-1, 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 675580-49-1, name is (6-Chloroimidazo[1,2-b]pyridazin-3-yl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

(6-Chloroimidazo[1,2-b]pyridazin-3-yl)methanol 72 (1 mmol) and the alkyl iodide (1.1 mmol) were dissolved in dry DMF (2 mL) and sodium hydride (60% disp, 1.1 mmol) added. After 2 h the mixture was poured into water and extracted (2×) with ethyl acetate. The combined organic layers were washed with 5% lithium chloride solution (5×), dried, concentrated and the residue purified by column chromatography (12 g ISCO column eluting with methylene chloride and a methanol/ammonia mixture (10:1); gradient 100% methylene chloride to 80% methylene chloride over 30 min at 25 mL/min) to provide the desired product 8.8a 6-Chloro-3-(methoxymethyl)imidazo[1,2-b]pyridazine was obtained as a yellow oil (100 mg, 51%); Rf=0.90 (CH2Cl2/MeOH/NH4OH, 160:18:2); 1H NMR (500 MHz, CD3OD) delta 8.05 (d, J=9.5 Hz, 1H), 7.81 (s, 1H), 7.34 (d, J=9.5 Hz, 1H), 4.85 (s, 2H), 3.41 (s, 3H).8b 6-Chloro-3-(ethoxymethyl)imidazo[1,2-b]pyridazine was obtained as a yellow oil (111 mg, 53%); Rf=0.90 (CH2Cl2/MeOH/NH4OH, 160:18:2); 1H NMR (500 MHz, CD3OD) delta 8.01 (d, J=9.5 Hz, 1H), 7.80 (s, 1H), 7.34 (d, J=9.5 Hz, 1H), 4.87 (s, 2H), 3.63 (quart, J=7.0 Hz, 2H), 1.21 (t, J=7.0 Hz, 3H).

According to the analysis of related databases, 675580-49-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALCON MANUFACTURING, LTD.; US2008/153813; (2008); A1;,
Alcohol – Wikipedia,
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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.64372-62-9, name is 2-Chloro-5-(trifluoromethyl)benzyl alcohol, molecular formula is C8H6ClF3O, molecular weight is 210.58, as common compound, the synthetic route is as follows.Safety of 2-Chloro-5-(trifluoromethyl)benzyl alcohol

Step 1 : Suzuki Coupling Reaction of Boronic Acid 5 and Aryl Chloride 13 to yield 6: A 3 M K2CO3 solution is prepared by adding 4.71 kg of solid K2CO3 to 10.3 L water. Cooling is applied to keep the solution at 20-25 0C. THF (12 L), aryl chloride 13 (2.69 kg), and boronic acid 5 (2.74kg) are added to the K2CO3 followed by a 1 L THF rinse. HPLC analysis is used to confirm the 1.00/1.00 ratio of 5/13. The solution is degassed by sparging with nitrogen gas for 70 min. The catalyst, 1,1 bis(di-tert- butylphosphino)ferrocene palladium dichloride (42g) is added as a solid and is followed by a degassed THF rinse (1.5 L). The organic layer turns dark brown immediately. The biphasic mixture is aged at 36-40C with vigorous stirring. After HPLC reveals complete conversion (15-18 h), the mixture is cooled to rt and the aqueous layer is removed. To the organic layer is added heptane (25.6L) and water (25.6 L) and the layers are cut. The organic layer is washed with water (19L). The organic layer is treated with 680 g Darco KB-B at rt for 60 min and filtered through solka-floc with a 10%THF/Heptane rinse (-15 L). The solvent is switched to heptane (-35 L) at -45-50 0C until <0.5v% of THF is left. More heptane is added to bring the total volume to -45-50 L. The solution is seeded with crystals obtained from earlier runs if no seed bed forms. The slurry is slowly cooled to rt and then to -15 0C. After aging at -15 0C for 1-2 h, after LC of the supernatant shows that there will be ~2g/l loss of the product in the supernatant, the slurry is filtered and the product is washed with cold heptane (-25 L), providing compound 6. At the same time, in my other blogs, there are other synthetic methods of this type of compound,64372-62-9, 2-Chloro-5-(trifluoromethyl)benzyl alcohol, and friends who are interested can also refer to it. Reference:
Patent; MERCK & CO., INC.; WO2007/5572; (2007); A1;,
Alcohol – Wikipedia,
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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 16700-55-3, name is (2,6-Dimethoxyphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of (2,6-Dimethoxyphenyl)methanol

To 15 ml of dichloromethane were added 1.1 g of 3-[bis(4-fluorophenyl)methyl]-4-piperidinone hydrochloride, 1.7 ml of isopropyl ethylamine and 0.6 g of 2, 6-dimethoxybenzyl alcohol and the mixture was stirred at room temperature.. Then, 0.8 ml of EPPA was added thereto and the mixture was allowed to stand at room temperature for 4 days.. The solvent was distilled off under reduced pressure, and the residue was purified by subjecting it to silica gel column chromatography (40 g, ethyl acetate: hexane = 1: 1) to obtain 0.88 g of the title compound (yield: 60%). mp 125-126C. IR (KBr).. 1705, 1595, 1505, 1470, 1250, 1215, 1110, 830, 555, 525 cm-1.

With the rapid development of chemical substances, we look forward to future research findings about 16700-55-3.

Reference:
Patent; Takeda Chemical Industries, Ltd.; EP1460062; (2004); A1;,
Alcohol – Wikipedia,
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