ChemicalBook CAS DataBase List 3-Bromophenylacetic acid

3-Bromophenylacetic acid synthesis

11synthesis methods

Product Name:3-Bromophenylacetic acid
CAS Number:1878-67-7
Molecular formula:C8H7BrO2
Molecular Weight:215.04

1,1'-Bis(diphenylphosphino)ferrocene (8.9 mg, 0.016 mmol, 4 mol%) and the corresponding hydrazone (0.40 mmol, 1.0 eq. of non-liquid hydrazone) were loaded into dry Schlenk tubes (25 mL) containing a stirring bar, and the reaction tubes were transferre

2142-63-4 Synthesis

2142-63-4
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1878-67-7
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Yield:1878-67-7 92.3%

Reaction Conditions:

Stage #1:1-(3-Bromophenyl)ethanone with 4-methyl-morpholine;sulfur for 14 h;Reflux;
Stage #2: with sulfuric acid;acetic acid in water at 20 - 30; for 6 h;Reflux;

Steps:

1.1 first stepPreparation of 3-bromo-phenylacetic acid (2)
In 1000ml three-necked flask of sublimed sulfur were added 24g (0.75mol), 100g3- bromoacetophenone (0.5mol) and 65.4g (0.75mol) morpholine was stirred at reflux for 14 hours. Cooling to 20 ~ 30 , stirring joined by glacial acetic acid 260ml, 75ml and 52ml distilled water mixed with concentrated sulfuric acid solution dubbed refluxing was continued for 6 hours. The reaction mixture was poured into ice water, stirring to brown solid precipitated was filtered. The solid was dissolved 300ml20% aqueous sodium hydroxide solution and filtered. The filtrate was placed in an ice bath, 2mol / L of hydrochloric acid to adjust pH = 1 ~ 2, crystallization, filtration, 60 dried to give 99.2g of yellow solid 2, a yield of 92.3%.

References:

Weihai Disu Pharmaceutical Co., Ltd.;Weihai Dijia Pharmaceutical Co., Ltd.;Liu, Qingchun;Chen, Huilai;Sun, Jian;Wang, Huabing;Meng, Cunzhi;Song, Gaofeng CN105348195, 2016, A Location in patent:Paragraph 0005; 0015

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201230-82-2 Synthesis