Month: June 2021

Electric Literature of 20712-12-3, Adding some certain compound to certain chemical reactions, such as: 20712-12-3, name is (2-Amino-5-bromophenyl)methanol,molecular formula is C7H8BrNO, 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 20712-12-3.

(l) To a mixture of lithium aluminum hydride (2.6 g, 69 mmol) in diethyl ether (54 ml) was added dropwise 5-bromoanthranillic acid methyl ester (6.3 g, 27 mmol) in diethyl ether (54 ml) at Ot). The mixture was stirred at O1C for 3 hours. Then water (2.6 ml), 15 wtpercent aqueous solution of sodium hydroxide (2.6 ml) and water (7.8 ml) was addedsequentially at O1C. The mixture was filtrated through a pad of Celite, and concentrated in vacuo. The residue was dissolved into tetrahydrofuran (160 ml), and triethylamine (15 g, 150 mmol) was added. The mixture was cooled to Ot, and trichloromethyl chloroformate (2.9 g, 15 mmol) was added. The mixture was stirred at room temperature for 4 hours. The mixture was partitioned between water and ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and concentrated in vacuo to afford crude product. This crude product was washed with diethyl ether to afford6-bromo-l,4-dihydro-2H”3,l-benzoxazin-2-one as a colorless solid (4.7g, 21 mmol, 77percent).

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. 20712-12-3, (2-Amino-5-bromophenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MITSUBISHI TANABE PHARMA CORPORATION; SANOFI-AVENTIS; NAKAYAMA, Kazuki; SAKAI, Daiki; WATANABE, Kazutoshi; KOHARA, Toshiyuki; ARITOMO, Keiichi; WO2011/19090; (2011); A1;,
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Synthetic Route of 50595-15-8, 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 50595-15-8, name is tert-Butyl 2-hydroxyacetate. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 5-bromo-3H-oxazolo[4,5-b]pyridin-2-one (300 mg, 1.4 mmol) in THF (5 mL) was added tert-butyl 2-hydroxyacetate (553.23 mg, 4.19 mmol), PPh3 (731.97 mg, 2.79 mmol) and then DIAD (564.31 mg, 2.79 mmol). The resulting mixture was stirred at 25 °C under N2 for 16 hours to give a solution. The reaction solution was concentrated to give a residue. Water (20 mL) was added to the residue, and the mixture was extracted with EtOAc (20 mL x 2). The combined organic layer was washed with brine (20 mL x 2), dried over anhydrous Na2SC>4, filtered and concentrated to give the crude product. The crude product was purified by flash chromatography on silica gel (EtOAc in PE = 0percent to 10percent to 30percent) to give the product (400 mg, 1.22 mmol, 87percent yield) as a solid. *H NMR CDC13, 400MHz deltaH = 7.33 – 7.29 (m, 1H), 7.27 – 7.24 (m, 1H), 4.55 (s, 2H), 1.48 (s, 9H).

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 50595-15-8, tert-Butyl 2-hydroxyacetate.

Reference:
Patent; PRAXIS PRECISION MEDICINES , INC.; REDDY, Kiran; MARTINEZ BOTELLA, Gabriel; GRIFFIN, Andrew, Mark; MARRON, Brian, Edward; (244 pag.)WO2018/148745; (2018); 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.349-75-7, name is (3-(Trifluoromethyl)phenyl)methanol, molecular formula is C8H7F3O, molecular weight is 176.14, as common compound, the synthetic route is as follows.SDS of cas: 349-75-7

General procedure: 1-methyl-3-[(3-cyanophenylmethoxy)methyl]-2(1H)-pyridinone, 12a. To a 0 C suspension of sodium hydride (41 mg, 60% suspension in mineral oil, 1.01 mmol), in THF (3 mL) was added 3-cyanobenzyl alcohol (100 mg, 0.75 mmol). After the mixture was stirred for 1 h at 0 C, 3-(bromomethyl)-1-methylpyridin-2(1H)-one3 (152 mg, 0.75 mmol) in THF (3mL) was added dropwise. The reaction mixture was slowly allowed to warm to room temperature and stirred for additional 3 h before diluting with saturated aqueous ammonium chloride. After extraction with ethyl acetate, the combined organics were washed with brine, concentrated invacuo and purified by column chromatography using 5:95 MeOH/DCM to get title compound as a colorless soild (136 mg, 71 %).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,349-75-7, (3-(Trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Khatri, Buddha B.; Vrubliauskas, Darius; Sieburth, Scott McN.; Tetrahedron Letters; vol. 56; 30; (2015); p. 4520 – 4522;,
Alcohol – Wikipedia,
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Synthetic Route of 349-75-7, 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.349-75-7, name is (3-(Trifluoromethyl)phenyl)methanol, molecular formula is C8H7F3O, molecular weight is 176.14, as common compound, the synthetic route is as follows.

Sequentially capturing meso-Co-N / C (800) (35mg, 0.25mol% Co), 3- trifluoromethyl-benzyl alcohol (176mg, 1mmol), a concentration of 28 mass% aqueous ammonia (280 L) was added to the reaction flask 10ml and tert-amyl alcohol was added 1ml of solvent placed in the reaction vessel, the oxygen charged to 1Mpa, placed in an oil bath of 130 and then detecting the extent of reaction by GC-MS.After completion of the reaction, the biphenyl internal standard was added, the product was analyzed 3-trifluoromethyl-benzonitrile quantitative yield by GC.The reaction 24h, 3- trifluoromethyl-benzonitrile in 83% yield, selectivity of 99%.

The chemical industry reduces the impact on the environment during synthesis 349-75-7, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Dalian Institute of Chemical Physics; Gao Shuang; Shang Sensen; Wang Lianyue; Lv Ying; (7 pag.)CN106883143; (2017); A;,
Alcohol – Wikipedia,
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Electric Literature of 456-47-3 ,Some common heterocyclic compound, 456-47-3, molecular formula is C7H7FO, 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.

General procedure: A mixture of H2O (5 mL) and CH2Cl2 (5 mL) wasadded to the chlorinated polymeric beads (2 g). (The unchlorinated beads were obtained from HaloSource, Inc. The unchlorinated beads were chlorinated by soaking the beads in bleach solution, with pH adjusted to 7 by additionof AcOH, for an hour. Then, the chlorinated beads were filtered and dried in air.) After addition of TEMPO (10 mg,0.064 mmol) and benzyl alcohol (0.2 g, 1.8 mmol), NaHCO3(0.5 g) was added to the mixture. The mixture was stirred at r.t. for 3 h and filtered. The residue on the filter paper was washed with H2O (20 mL) and CH2Cl2 (10 mL), and the organic phase of the filtrate was separated, dried over MgSO4, and filtered. The solvent was removed under vacuum to obtain benzaldehyde.

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. 456-47-3, 3-Fluorobenzyl alcohol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Akdag, Akin; Oeztuerk, Perihan; Synlett; vol. 24; 18; (2013); p. 2451 – 2453;,
Alcohol – Wikipedia,
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Synthetic Route of 3344-77-2, 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.3344-77-2, name is 12-Bromododecan-1-ol, molecular formula is C12H25BrO, molecular weight is 265.23, as common compound, the synthetic route is as follows.

Example 2 Preparation of (12-bromododecyloxy)(tert-butyl)dimethylsilane (4) Tert-butyldimethylsilyl chloride (5.61 g; 37.3 mmol; 1.5 eq.) and imidazole (2.54 g; 37.3 mmol; 1.5 eq.) are added to a solution of 12-bromododecan-1-ol (6.6 g; 24.9 mmol; 1 eq.) in dichloromethane (60 ml) at room temperature. After 4 h, the reaction mixture is poured into a saturated solution of NH4Cl (100 ml) and then extracted with ether (3*100 ml). The organic phase is washed with a saturated solution of NaCl, dried on MgSO4, filtered then evaporated. The crude reaction product is purified by silica gel chromatography (eluent: hexane-AcOEt: 95-5) to yield 9.17 g of a colorless oil. Yield: 99percent Empirical formula: C18H39BrOSi

Statistics shows that 3344-77-2 is playing an increasingly important role. we look forward to future research findings about 12-Bromododecan-1-ol.

Reference:
Patent; Centre National de la Recherche Scientifique(CNRS); Universite de Luxembourg; US2010/48731; (2010); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 1562-00-1, Sodium isethionate, 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, COA of Formula: C2H5NaO4S, blongs to alcohols-buliding-blocks compound. COA of Formula: C2H5NaO4S

Example 9; Preparation of N-Methyl vinyl sulfonamide; PART A: A mixture of isethionic acid sodium salt (0.250 Kg, 1689 mmol) was taken inDMF (0.32L) and dichloromethae (0.3L). To this mixture thionyl chloride (0.375L, 5186mmol) was added dropwise at 20-30C. The reaction mixture was heated slowly from 30-60 “C. After completion of the reaction 3.5 lit of chilled water was added. The reaction mixture was extracted with 3×0.5L dichloromethane. Then dichloromethane was distilled out from the reaction mixture to get an oil. [ Yield 0.250Kg, 90%] which was distilled under vacuum to get pure chloroethane sulfonyl chloride. (0.225kg, 90%).

The synthetic route of 1562-00-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; USV LIMITED; WO2009/118753; (2009); A2;,
Alcohol – Wikipedia,
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Application of 162744-59-4, 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 162744-59-4 as follows.

A solution of 5-Bromo-2-hydroxymethyl-1, 3-difluoro-benzene (0. 89g, 4.0 mmol) and 30 wt% of hydrogen bromide in acetic acid was stirred at room temperature for 90 minutes before it was poured into 80 ml of water. The mixture was extracted with pentane (3 X 50 ML) and the combined organic layers were washed with water (3 X 20 ML), dried over MGSO4 and concentrated at low pressure to afford the desired product (10.0 g, 98% YIELD). 1H NMR (CDC13) 8 : 4.47 (s, 2H), 7.09-7. 10 (m, 1H), 7. 12-7. 13 (m, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,162744-59-4, its application will become more common.

Reference:
Patent; PFIZER INC.; WO2004/74270; (2004); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. 14320-38-8, name is Cyclopent-3-enol. A new synthetic method of this compound is introduced below., COA of Formula: C5H8O

Cyclopent-3-en-1-ol (10 g, 119 mmol, commercially available from, for example, Fluorochem) was dissolved in a mixture of DMF (100 mL) and THF (50 mL) and cooled in an ice bath under nitrogen, then NaH (60% suspension in mineral oil, 5.71 g, 143 mmol) was added in small portions and the mixture stirred for 30 min, before addition of MeI (9.66 mL, 155 mmol). The resulting suspension was stirred at 0 C for 2 h, then added to water (500 mL) and extracted with ether (500 mL). The organic layer was washed with water (2 x 200 mL) and brine (200 mL), dried and evaporated in vacuo to give the desired product as a pale yellow liquid, which was carried through to subsequent reactions without further purification. (0571) 1H NMR (400 MHz, CDCl3) delta ppm 5.61 – 5.82 (m, 2 H) 4.13 (dt, J=6.72, 3.48 Hz, 1 H) 3.35 (s, 3 H) 2.59 (dd, J=15.77, 6.72 Hz, 2 H) 2.32 – 2.47 (m, 2 H)

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, 14320-38-8, Cyclopent-3-enol.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; ATKINSON, Stephen John; DEMONT, Emmanuel Hubert; HARRISON, Lee Andrew; LIWICKI, Gemma Michele; LUCAS, Simon Christopher Cranko; PRESTON, Alexander G; SEAL, Jonathan, Thomas; WALL, Ian David; WATSON, Robert J; (0 pag.)WO2018/158212; (2018); A1;,
Alcohol – Wikipedia,
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Electric Literature of 929-06-6, 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. 929-06-6, name is 2-(2-Aminoethoxy)ethanol, molecular formula is C4H11NO2, 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.

PREPARATION 7: T-BUTYL 2-(2-HYDROXYETHOXY)ETHYLCARBAMATE To a single-neck flask was added 2-(2-aminoethoxy)ethanol (10.500 g). Tetrahydrofuran (25 mL) was added to dissolve2-(2-aminoethoxy)ethanol. Anhydrous sodium carbonate (5.300 g) was dissolved in distilled water (30 mL). The solution was added into the single-neck flask and cooled in an ice bath. Di-t-butyl dicarbonate (28.340 g) was dissolved in tetrahydrofuran (70 mL). The resultant solution was slowly dropwise added in the reaction system (for about 1 hr). After the addition, the mixture was stirred for 1.5 hr. After the reaction was completed, the reaction solution was filtered by suction. The filter cake was washed with tetrahydrofuran twice and then discarded. The filtrate was concentrated, then dissolved in ethyl acetate (150 mL) and distilled water (100 mL). The solution was mixed and then stood to separate. The aqueous phase was washed again with ethyl acetate (100 mL * 2) twice. All the organic phases were combined, dried over MgSO4, filtered and concentrated to give the target compound.

According to the analysis of related databases, 929-06-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Tianjin Hemay Bio-Tech Co., Ltd.; ZHANG, Hesheng; HUO, Aihong; LI, Zhenzhong; EP2824108; (2015); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts