HRID1972435

反应详情

EQUATION

反应方程式

HRID 1972435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Osmium tetroxide (4 wt % solution with water, 4.3 mL, 0.70 mmol) was added to a stirring mixture of 1-bromo-4-(1-(trifluoromethyl)ethenyl)benzene (3.5 g, 14 mmol), 4-methylmorpholine N-oxide (1.8 g, 15 mmol), acetone (14 mL), and water (14 mL) at room temperature. After 21 h, Na2SO3 (8.8 g, 70 mmol) was added, the mixture was filtered. Silica gel (20 g) was added to the filtrate, and the volatiles were removed in vacuo. The residue was purified via column chromatography (5% MeOH in CH2Cl2) to afford 2-(4-bromophenyl)-3,3,3-trifluoro-1,2-propanediol (3.0 g) as an off-white solid.

WORKUP

后处理

  1. filtrationthe mixture was filtered
  2. additionSilica gel (20 g) was added to the filtrate
  3. customthe volatiles were removed in vacuo
  4. customThe residue was purified via column chromatography (5% MeOH in CH2Cl2)