HRID347156
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
7.4 g (23.17 mmol) 3-(4-Bromo-phenyl)-6-methoxy-benzo[b]thiophene in 47 ml acetic acid were treated with 27 ml (62% aq) HBr at 125° C. for 4 h. The solution was concentrated in vacuo and the residue was dissolved in NaHCO3 and EtOAc. Prior to extraction with EtOAc the pH was adjusted with 2M NaOH (pH 8). The combined organic phases were washed with brine and dried with Na2SO4. Trituration with hexane gave 6.96 g (98%) 3-(4-Bromo-phenyl)-benzo[b]thiophen-6-ol as light green solid, MS: 304 (M, 1Br).
WORKUP
后处理
- concentrationThe solution was concentrated in vacuo
- dissolutionthe residue was dissolved in NaHCO3
- extractionPrior to extraction with EtOAc the pH
- washThe combined organic phases were washed with brine
- dry with materialdried with Na2SO4