HRID1183530

反应详情

EQUATION

反应方程式

HRID 1183530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-(4-Bromo-phenyl)-cyclopropanecarboxylic acid (22 g, 91.3 mmol) and SOCl2 (13.6 mL, 183 mmol) in CH2Cl2 were heated together for 1.5 hours then evaporated to afford a dark oil. This oil was added via syringe over 30 minutes to a mixture of MeSO2NH2 (19 g, 200 mmol) in THF (250 mL) that was pre-treated at room temperature with NaH (60% in oil; 8.0 g, 200 mmol) for 1.5 hours. After a further 20 minutes, the mixture was poured into water, acidified and extracted with CH2Cl2, washed with water (2×) and evaporated to ˜100 mL. Hexane (300 mL) was added and the product collected by filtration to yield the title compound (25 g).

WORKUP

后处理

  1. customthen evaporated
  2. customto afford a dark oil
  3. extractionextracted with CH2Cl2
  4. washwashed with water (2×)
  5. customevaporated to ˜100 mL
  6. additionHexane (300 mL) was added
  7. filtrationthe product collected by filtration