Month: June 2021

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. 558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, 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. Product Details of 558-42-9

Step 1: Methyl 1H-pyrazole-3-carboxylate (2.52 g, 20 mmol, 1 equiv.) was dissolved in DMF (20 mL). K2CO3 (5.53 g, 40 mmol, 2 equiv.) was added, followed by 1-chloro-2-methyl- 2-propanol (2.67 mL, 26 mmol, 1.3 equiv.). The reaction mixture was heated to 80 °C for 40 hours and cooled to room temperature. The reaction mixture was poured into water, extracted with EtOAc, and the combined organic extracts were washed with water and brine. The organic layer was concentrated, and the crude residue was purified on SiO2 (25 100percent EtOAc/Hexanes) to afford the title compound as a colorless oil that solidified upon standing (2.08 g, 53percent yield).

With the rapid development of chemical substances, we look forward to future research findings about 558-42-9.

Reference:
Patent; ARCUS BIOSCIENCES, INC.; LELETI, Manmohan Reddy; MILES, Dillon Harding; POWERS, Jay Patrick; ROSEN, Brandon Reid; SHARIF, Ehesan Ul; (109 pag.)WO2018/213377; (2018); A1;,
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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. 171011-37-3, name is (4-Bromo-1,2-phenylene)dimethanol. A new synthetic method of this compound is introduced below., SDS of cas: 171011-37-3

After dissolving Compound 3 (5.2 g, 23.9 mmol) in methylene chloride (50 milliliter), followed by adding N-bromosuccinimide (12.8 g, 71.7 mmol) at room temperature, and then the resultant solution was stirred for 6 hours. Water (200 milliliter) was poured in the resultant reaction solution, and the deposited solid was washed by ethanol, and as a result, Compound 4 was obtained. Product Amount: 6.9 g, Yield: 84 %

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, 171011-37-3, (4-Bromo-1,2-phenylene)dimethanol.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1659129; (2006); A1;,
Alcohol – Wikipedia,
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Reference of 14320-38-8, 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.14320-38-8, name is Cyclopent-3-enol, molecular formula is C5H8O, molecular weight is 84.12, as common compound, the synthetic route is as follows.

To a solution of cyclopent-3-en-1-ol (compound 32a, 5.0 g, 59.4 mmol) in THF (100.0 ml) was added NaH (3.1 g, 77.2 mmol) in portions at 0 oC. The reaction was stirred at the same temperature for 30 minutes, then BnBr (10.2 g, 59.4 mmol) was added dropwise. The reaction was warmed to room temperature and stirred for 12 hours. The reaction was quenched with H2O (300 mL) and extracted with EtOAc twice (200 mL). The combined organic layer was dried over Na2SO4, concentrated to give compound 32b (12.5 g, crude) as a brown oil.

Statistics shows that 14320-38-8 is playing an increasingly important role. we look forward to future research findings about Cyclopent-3-enol.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; HU, Taishan; KOU, Buyu; LIN, Xianfeng; LIU, Haixia; ZHANG, Zhisen; (152 pag.)WO2018/11160; (2018); A1;,
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Related Products of 61367-62-2, 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. 61367-62-2, name is 4-Bromo-3,5-dimethoxybenzyl alcohol. A new synthetic method of this compound is introduced below.

To a round bottom flask was added (4-bromo-3,5-dimethoxy-phenyl)methanol (Compound 10, 0.5 g, 2.02 mmol) and dichloromethane (15 mL). The reaction was cooled to 0 °C and diethylaminosulfur trifluoride (0.360 g, 2.23 mmol) was added. The reaction was allowed to warm to room temperature and stir for 1 hour. The reaction was quenched using saturated sodium bicarbonate, the layers were separated and the organic layer was dried using sodium sulfate, filtered and concentrated in vacuo. The resulting solid was purified on silica gel using ethyl acetate and hexanes as eluent. Product, 2-bromo-5-(fluoromethyl)-l,3- dimethoxybenzene, (Compound 14, 0.171 g, 33.9percent yield) was isolated as a pale yellow solid. LC-MS: tR=2.23 min; m+H=249.0, 251.0 (bromine isotopes).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,61367-62-2, 4-Bromo-3,5-dimethoxybenzyl alcohol, and friends who are interested can also refer to it.

Reference:
Patent; SAINT LOUIS UNIVERSITY; WASHINGTON UNIVERSITY; RUMINSKI, Peter, G.; MEYERS, Marvin, L.; HEIER, Richard, F.; RETTIG, Michael, P.; DIPERSIO, John; (139 pag.)WO2018/85552; (2018); A1;,
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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. 27871-49-4, name is (S)-Methyl 2-hydroxypropanoate, molecular formula is C4H8O3, 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. COA of Formula: C4H8O3

a solution of methyl (2S)-2-hydroxypropanoate (5 g, 48.03 mmol, 1.00 eq.) and 1H-imidazole (4.9 g, 71.98mmol, 1.50 eq.) in dichloromethane (100 mL) was placed into a 250-mL round-bottom flask. This was followed by the addition of a solution of tert-butyl(chloro)dimethylsilane (8.69 g, 57.66 mmol, 1.20 eq.) in dichloromethane (50 mL) dropwise with stirring at 0C. The resulting solution was stirred for 2 hours at room temperature. The reaction was then quenched by the addition of 80 mL of water/ice and extracted with dichloromethane (3×50 mL). The resultingmixture was washed with brine (2×100 mL), dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 8 g (76%) of methyl (2S)-2-[(tert- butyldimethylsilyl)oxy]propanoate as a colorless liquid.

With the rapid development of chemical substances, we look forward to future research findings about 27871-49-4.

Reference:
Patent; BASTOS Cecilia M.; MUNOZ Benito; TAIT Bradley; WO2015/196071; (2015); A1;,
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Reference of 3513-81-3, 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 3513-81-3 as follows.

2-METHYLENE-1, 3-propanediol (2.20 g, 25.0 MM) was stirred in dichloromethane (20 ML) and cooled to 0 °C. A 1 N solution of diethylzinc in hexanes (3.40 g, 27.5 MM) was added followed by a solution OF 4-BROMO-3-FLUORO-N-HYDROXYBENZENECARBOXIMIDOYL chloride (6.30 g, 25.0 MM) in dichloromethane (40 mL). The reaction was allowed to warm to room temperature and was complete after four hours. The solution was diluted with ammonium chloride and extracted using dichloromethane. The organic layer was dried (magnesium sulfate), filtered and concentrated to give the desired product as a yellow solid (4.72 g). MS (ESP : 305 (MH+) for CLLHLLBREINO3 300 MHz NMR (DMSO-D 6 : 3.29 (s, 2H); 3.55 (s, 2H); 3.57 (s, 2H) ; 5.10 (t, 2H); 7.52 (d, 1H); 7.68 (d, 1H); 7.86 (t, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3513-81-3, its application will become more common.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/48392; (2004); A1;,
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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. 1562-00-1, name is Sodium isethionate, molecular formula is C2H5NaO4S, 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. SDS of cas: 1562-00-1

Approximately 1.7 g of Compound A was added to a bottle and dissolved in 34 mL of acetone, concentration of 50 mg/mL. 400 pL (20 mg of freebase) of the stock solution was then dispensed into 84 vials and the acetone allowed to evaporate. 1M stock solutions of each counterion were prepared in either THF, ethanol or water, where appropriate as outlined in Table 27. L-aspartic acid was added as neat counterion due to low solubility. 1.05 equivalents of each counterion was added at room temperature and observations made. 2-hydroxy ethanesulfonic acid was supplied as a sodium salt and had 1.05 equivalents of HC1 added after counterion addition. All samples were then temperature cycled using the following procedure: a) Heat to 40 C, hold for 1 hour; b) Cooled to room temperature, hold for 3 hours; c) Heat to 40 C, hold for 1 hour; and d) Samples were held at 5 C overnight.All samples displaying solutions had the lids removed from the vials and were allowed to evaporate at ambient temperature. Samples with solid material had the mother liquor removed and the solids analyzed by XRPD. The mother liquor was transferred to a new sample vial and stored at 5 C to allow for further precipitation. The analyzed solids on the XRPD plate were exposed to 40 C/75 % RH conditions for 6 hours before analysis by XRPD. Table 27. Solvents Used to make Acid Stock Solutions

With the rapid development of chemical substances, we look forward to future research findings about 1562-00-1.

Reference:
Patent; ALDEYRA THERAPEUTICS, INC.; MACHATHA, Stephen, Gitu; LOUGHREY, Jonathan, James; MCLACHLAN, Hannah, Ruth; SNEDDON, Gregor; (194 pag.)WO2020/33344; (2020); A1;,
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Electric Literature of 3279-95-6, 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. 3279-95-6, name is 2-(Aminooxy)ethanol, molecular formula is C2H7NO2, 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.

Starting from intermediate 1.i (0.103 g; 0.2 mmol) and 2-aminooxyethanol (0.017 g; 0.221 mmol), the solutionwas stirred for th. The reaction mixture was directly purified by prep-HPLC (Method 1) to afford the titlecompound (0.084 g, 86% yield) as a white amorphous solid.MS1 (ESI, m/z): 485.1 [M+H*] for CigH2aN4O7So; tr = 0.65 min.

According to the analysis of related databases, 3279-95-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; IDORSIA PHARMACEUTICALS LTD; DIETHELM, Stefan; MATHIEU, Gaelle; PANCHAUD, Philippe; SURIVET, Jean-Philippe; TIDTEN-LUKSCH, Naomi; (123 pag.)WO2019/38362; (2019); A1;,
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Electric Literature of 455-01-6, 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. 455-01-6, name is 2-(3-(Trifluoromethyl)phenyl)ethanol. A new synthetic method of this compound is introduced below.

Reference Example 19-1 [3-(Trifluoromethyl)phenyl]acetaldehyde To a solution of 3-(trifluoromethyl)phenethyl alcohol (2.00 g) in chloroform (50.0 mL), Dess-Martin periodinane (4.70 g) was added under cooling with ice. After being brought to room temperature, the reaction mixture was stirred for an hour. Subsequently, a saturated aqueous solution of sodium hydrogencarbonate (25.0 mL) and a saturated aqueous solution of sodium thiosulfate (25.0 mL) were added and the mixture was vigorously stirred for an hour. After phase separation, the organic layer was dried over anhydrous magnesium sulfate, the desiccant was removed by filtration, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate = 98:2-85:15) to give the titled compound as a pale yellow oil (1.19 g). 1H NMR (300 MHz, CHLOROFORM-d) delta ppm 3.79 (s, 2 H) 7.36 – 7.62 (m, 4 H) 9.77 – 9.81 (m, 1 H). MS ESI/APCI Dual nega: 187[M-H]-.

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:
Patent; Taisho Pharmaceutical Co., Ltd.; TAKAYAMA, Tetsuo; SHIBATA, Tsuyoshi; SHIOZAWA, Fumiyasu; KAWABE, Kenichi; SHIMIZU, Yuki; HAMADA, Makoto; HIRATATE, Akira; TAKAHASHI, Masato; USHIYAMA, Fumihito; OI, Takahiro; SHIRASAKI, Yoshihisa; MATSUDA, Daisuke; KOIZUMI, Chie; KATO, Sota; EP2881384; (2015); A1;,
Alcohol – Wikipedia,
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Synthetic Route of 6329-73-3, 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. 6329-73-3, name is 1-(Benzo[d][1,3]dioxol-5-yl)ethanol, molecular formula is C9H10O3, 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.

General procedure: To a stirred solution of alcohol (1 equiv) in dry DCM (10 to 20 mL), thionyl chloride (1 .7 to 3 equiv) was added slowly at 0 C. The reaction mixture was warmed to rt and was refluxed for 1 h. The reaction mixture was concentrated under vacuum and the resulting residue was diluted with DCM (20 to 50 mL). The DCM layer was washed with water (5 to 10 mL), brine solution (5 to 10 mL), dried over anhydrous Na2SO4 and concentrated under vacuum to give chloro compound.

According to the analysis of related databases, 6329-73-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASCENEURON SA; QUATTROPANI, Anna; KULKARNI, Santosh S.; GIRI, Awadut Gajendra; (243 pag.)WO2016/30443; (2016); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts