HRID1857081

反应详情

EQUATION

反应方程式

HRID 1857081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

Acetophenone (10.1 g; 0.084 mol) and MCPC (25.2 g; 0.25 mol; 3 equiv) were dissolved in DMSO (46.1 g). Sodium methoxide (9.1 g; 0.168 mol; 2.0 equiv) was added slowly while maintaining the temperature below 30° C. The reaction mixture was then heated to 40° C. for 5 h. Heptane (100 mL) was added followed by sufficient 20% aqueous HCl such that the pH was less than 5. The mixture was stirred for 15 min and then allowed to settle. The lower aqueous layer was decanted and discarded. The upper organic layer was washed with 40 mL of water, and the solvent was stripped to afford 14 g of crude 8, which was 97.2% pure by GC (area %) to afford an 86% yield of 8.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature below 30° C
  2. customThe lower aqueous layer was decanted
  3. washThe upper organic layer was washed with 40 mL of water
  4. customto afford 14 g of crude 8, which