Month: May 2021

Related Products of 346-06-5, 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. 346-06-5, name is (2-(Trifluoromethyl)phenyl)methanol. A new synthetic method of this compound is introduced below.

a) A solution of 30 ml of phosphorus tribromide in 60 ml of absolute toluene was added dropwise at 20°-30° C. to a solution of 14 g of o-trifluoromethylbenzyl alcohol in 80 ml of absolute toluene. Subsequently, the reaction mixture was stirred at room temperature for 2 hours, the toluene was distilled under reduced pressure, the residue was dissolved in methylene chloride, treated with water and the mixture was adjusted to pH 8.0 with potassium hydrogen carbonate. The aqueous phase was extracted three times with CH2 Cl2 and the organic phases were washed twice with water and once with saturated NaCl solution, dried over Na2 SO4 and evaporated under reduced pressure. o-Trifluoromethylbenzyl bromide was obtained as the residue.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,346-06-5, (2-(Trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Hoffmann-La Roche Inc.; US5270313; (1993); A;,
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Synthetic Route of 50595-15-8, 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. 50595-15-8, name is tert-Butyl 2-hydroxyacetate, molecular formula is C6H12O3, 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: The title compound was prepared according to the General procedure A using tert-butyl glycolate and intermediate A as starting materials. The crude product was purified by FCC (0 to 100 percent DCM in hexane). Y = 65 percent. MS ES+ ([M+Na]+): 354.4. NMR (400 MHz, DMSO-d6) delta 9.13 (s, 1H), 6.95 (s, 1H), 4.48 (s, 2H), 2.81 (t, J= 7 Hz, 4H), 2.72 (t, J= 7 Hz, 4H), 2.03 – 1.91 (m, 4H), 1.43 (s, 9H). The a-hydroxy ester or a-hydroxy acid (1 eq.) was dissolved in ACN (2 ml/mmol of a- hydroxy ester or a-hydroxy acid) and the solution was cooled down to 0° C. TEA (1 eq.) was added followed by dropwise addition of the isocyanate (1.2 eq.). The reaction mixture was allowed to warm up to room temperature and stirring was continued for 15 h under Ar. The reaction mixture was diluted with DCM and the solution was washed with 1M HCl. The aqueous layer was extracted twice with DCM and the combined organic layers were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude product was purified by FCC (DCM or EtOAc gradient in hexane) or by preparative reverse-phase HPLC (ACN water, 0.1 percent formic acid buffer).

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; NODTHERA LIMITED; BOCK, Mark G.; WATT, Alan Paul; PORTER, Roderick Alan; HARRISON, David; (229 pag.)WO2019/25467; (2019); A1;,
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Application of 504-63-2, 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. 504-63-2, name is 1,3-Propanediol, molecular formula is C3H8O2, 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.

(1) Put 440kg of 1,3-propanediol, 600kg of hydrochloric acid, and 3kg of benzenesulfonic acid into a 2000L glass-lined kettle with a stirring and reflux condensing device, heat up to 90 C with stirring, and keep the reaction warm;(2) After holding for 3 hours, lower the temperature of the kettle to 50 C, then put 460kg of hydrochloric acid into the kettle, continue to warm to 90 C and keep the reaction for 10 hours. The temperature of the kettle is sampled for GC analysis. When the content reaches 80%, the feed liquid is poured into the distillation kettle, and 150 kg of toluene is poured into the distillation kettle to carry out the reaction of heating and refluxing with water;(3) After the reaction with water is completed, the temperature of the kettle is reduced to room temperature, and sodium bicarbonate is added to neutralize the oil phase in the kettle to neutrality, and the salt formed by the neutralization and excess sodium bicarbonate are filtered;(4) The filtered oil phase is pumped into the rectification kettle, and the solvent toluene is concentrated under normal pressure. After the toluene is collected, the product is rectified by high vacuum. The rectified fraction is put into the reaction kettle to continue the reaction.The content detected by GC gas chromatography was 99.3%, and the product yield was 96%.

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 504-63-2, 1,3-Propanediol.

Reference:
Patent; Zouping Mingxing Chemical Co., Ltd.; Chen Qiang; Zhang Peng; Zhang Junling; Cao Xinming; Sun Fantong; Wang Tao; Du Xiaoyang; (6 pag.)CN110668918; (2020); A;,
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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.37585-25-4, name is (2-Amino-5-chlorophenyl)methanol, molecular formula is C7H8ClNO, molecular weight is 157.6, as common compound, the synthetic route is as follows.Recommanded Product: (2-Amino-5-chlorophenyl)methanol

General procedure: To a solution of 1a (1.2 g, 7.61 mmol) in CH2Cl2 (20 mL) was added MnO2 (2.6 g, 30.1 mmol) and stirred at rt under an Ar atmosphere. After 23 h with stirring, the reaction mixture was filtrated and evaporated. The residue was crystallized from AcOEt to give 7a (1.0 g, 85%) as a yellow needle crystal.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,37585-25-4, (2-Amino-5-chlorophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Ida, Yoshihiro; Matsubara, Ayaka; Nemoto, Toru; Saito, Manabu; Hirayama, Shigeto; Fujii, Hideaki; Nagase, Hiroshi; Bioorganic and Medicinal Chemistry; vol. 20; 19; (2012); p. 5810 – 5831;,
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Electric Literature of 23147-58-2, Adding some certain compound to certain chemical reactions, such as: 23147-58-2, name is Glycerol aldehyde dimer,molecular formula is C4H8O4, 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 23147-58-2.

Example 2 Preparation of 4-Hydroxy-2-methyl-but-2-enoic acid ethyl ester 886 g (2.44 mol) of 2-(triphenyl-phosphanylidene)-propionic acid ethyl ester in methylene chloride (4 L) was added dropwise into a refluxing solution of glycoaldehyde dimer (140 g, 1.17 mol) in methylene chloride (6 L). After refluxing for 4 h, the solvent was evaporated. Resulting crude product was fractionated (bp 108-114 C. at 2 mmHg) to give 304 g (90%) pure product as an oil. 1H-NMR (300 Hz CDCl3) delta 6.88 (t, 1H, CH), 4.35 (d, 2H, CH2OH), 4.20 (q, 2H, OCH2), 1.85 (s, 3H, CH3), 1.30 (t, 3H, CH3).

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. 23147-58-2, Glycerol aldehyde dimer, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Lockwood, Samuel F.; Tang, Peng Cho; Nadolski, Geoff; Jackson, Henry L.; Fang, Zhiqiang; Du, Yishu; Yang, Min; Geiss, William; Williams, Richard; Burdick, David; Braun, Cristi L.; US2008/221377; (2008); 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. 37729-18-3, name is 2-([1,1′-Biphenyl]-4-yl)ethanol. A new synthetic method of this compound is introduced below., Quality Control of 2-([1,1′-Biphenyl]-4-yl)ethanol

4-Biphenylethanol (see Kawasaki et al., Tetrahedron: Asymmetry 2001, 12, 585-596) (1.47 g, 7.41 mmol) and CBr4 (1.12 equiv) were dissolved in CH2Cl2 (25 mL), the mixture was cooled to 0 C and triphenylphosphine (1.1 equiv) was added in small portions. The reaction mixture was warmed at room temperature and stirred for 1 h before the solvent was removed in vacuo. Flash chromatography (0-5% EtOAc-hexanes) yielded 4-(2-bromoethyl)biphenyl (1.59 g, 82%). The title compound was prepared from S7 (55 mg, 0.27 mmol) and 4-(2-bromoethyl)biphenyl (280 mg, 1.07 mmol) by using general procedure D. Flash chromatography (SiO2, 1.5 x 18 cm, 50-100% EtOAc-hexanes) afforded the title compound (38 mg, 40%) as a white solid: 1H NMR (CDCl3, 500 MHz) delta 8.84 (dd, IH, J = 0.7, 4.7 Hz), 8.29 (d, IH, J = 7.9 Hz), 7.92 (dt, IH, J = 1.7, 7.8 Hz), 7.57 (m, 2H), 7.53 (m, 3H), 7.42 (t, 2H, J = 7.7 Hz), 7.33 (m, 3H), 3.60 (t, 2H, J = 7.5 Hz), 3.19 (t, 2H, J = 7.5 Hz); 13C NMR (CDCl3, 150 MHz) delta 186.2, 165.3, 161.3, 150.9, 142.7, 141.0, 139.6, 139.0, 137.5, 129.0, 128.9, 127.5, 127.3, 127.2, 126.9, 124.2, 41.7, 29.1 ; HRMS-ESI-TOF m/z 356.1392 ([M+H]+, C22H17N3O2 requires 356.1393).

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, 37729-18-3, 2-([1,1′-Biphenyl]-4-yl)ethanol.

Reference:
Patent; THE SCRIPPS RESEARCH INSTITUTE; BOGER, Dale, L.; WO2010/5572; (2010); A2;,
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Synthetic Route of 101597-25-5 ,Some common heterocyclic compound, 101597-25-5, molecular formula is C17H16O3, 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.

Step 7 The product of Step 6 (4.8 g), was dissolved in dichloromethane (150 mL) in a 3-necked 100 mL round bottom flask, followed by addition of p-toluenesulfonic acid monohydrate (0.4 g). 1,1-Bis(4-methoxyphenyl)-2-propyn-1-ol (3.8 g) was added to the reaction mixture slowly. The mixture was stirred at room temperature. After one hour, more 1,1-bis(4-methoxyphenyl)-2-propyn-1-ol, (0.4 g) was added to the reaction mixture. After stirring for two hours, the reaction was worked up with the addition of saturated aqueous NaHCO3 (100 mL). The resulting organic layer was collected and dried over anhydrous MgSO4. The organic layer was concentrated under vacuum to provide product (8.7 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,101597-25-5, its application will become more common.

Reference:
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Application of 2807-30-9, Adding some certain compound to certain chemical reactions, such as: 2807-30-9, name is 2-Propoxyethanol,molecular formula is C5H12O2, 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 2807-30-9.

Using toluene with CEP-0 No.: toluene = 1: 2 (w / w) as a solvent, First in low temperature (-5 ~ 0 ) under the conditions of absorption of phosgene,Then the temperature of 0 ~ 5 dropping CEP-0 for photochemical reaction,The dropwise addition of phosgene continued to the end of the photochemical reaction,Slowly warmed to 30 , 30 under the conditions of nitrogen to catch the light, the light after the end of the transfer into the CEP-1No. drop tank spare.

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. 2807-30-9, 2-Propoxyethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Lier Chemical Co., Ltd.; Li Shihong; Cheng Ke; Wang Fuxiong; Zuo Xiang; (9 pag.)CN107311863; (2017); A;,
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Electric Literature of 161446-90-8, 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 161446-90-8, name is 3-Chloro-4-fluorobenzyl Alcohol. This compound has unique chemical properties. The synthetic route is as follows.

[00202] A solution of 3-chloro-4-fluorobenzaldehyde (3 g) in THF (40 ml) was added over 2 minutes to a stirred suspension of sodium borohydride (1.07 g) in methanol (40 ml) at 0 C. The mixture was allowed to warm to room temperature and then quenched with water. The resulting suspension was partitioned between water and diethyl ether and the combined organic extracts were dried and concentrated in vacuo. The residue was dissolved in dichloromethane (90 ml) and triphenylphosphine (4.62 g) and tetrabromomethane (6.64 g) were added at 0 C. The mixture was allowed to warm to room temperature overnight then concentrated in vacuo and the residue purified by column chromatography using iso-hexane as eluent to yield the desired product (3.57 g, 85%). NMR: delta 4.7 (s, 2H), 7.4 (m, 2H), 7.7 (m, 1H).

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 161446-90-8, 3-Chloro-4-fluorobenzyl Alcohol.

Reference:
Patent; AstraZeneca AB; US6737435; (2004); B1;,
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Application of 34231-22-6, 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. 34231-22-6, name is 3-(Aminomethyl)benzyl Alcohol, molecular formula is C8H11NO, 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.

Fmoc-OSu (38.6 g, 1 15 mmol) was added to a solution of [3-(amino- methyl)phenyl]methanol (S14, 16.5 g, 121 mmol) in THF (150 ml_), water (75 ml_) and sodium bicarbonate (20.3 g, 241 mmol) at room temperature (rt) and the reaction stirred overnight (o/n). At that point, a small sample was diluted with MeOH, acidified with a drop of HOAc, and analyzed by LC-MS, which showed the desired product with no Fmoc-OSu reagent. The reaction was acidified with 1 M HCI, diluted with ethyl acetate (EtOAc), and stirred for 2 h. The white solid was filtered off, washed well with water, then EtOAc, and air dried for 3 h until a constant weight was attained. The product thus obtained, Fmoc-S14 (15.3 g), was found by LC-MS to be free of identifiable organic impurities. The aqueous layer was extracted with EtOAc (2x). The combined organic layers were washed with H2O (2x) and brine, then dried over anhydrous MgSO4. The dessicant was removed by filtration and the filtrate concentrated under reduced pressure to give additional amounts of the desired product as a white solid (34.1 g). The combined solids were triturated with ethyl acetate at reflux for a few minutes, then o/n at rt to give Fmoc-S14 in 88% yield (38.1 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 34231-22-6, 3-(Aminomethyl)benzyl Alcohol.

Reference:
Patent; CYCLENIUM PHARMA INC.; WAHHAB, Amal; DUBE, Daniel; MACDONALD, Dwight; PETERSON, Mark L.; RICHARD, Luc; THOMAS, Helmut; (313 pag.)WO2018/232506; (2018); A1;,
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