HRID14482

反应详情

EQUATION

反应方程式

HRID 14482 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1-[2-Hydroxy-4-(4-methoxy-benzyloxy)-phenyl]-ethanone (9.11 g, 0.034 mol) is dissolved in dry dichloromethane (120 ml) under an atmosphere of dry argon. Triethylamine (5.14 ml, 0.037 mol) and 4-dimethylaminopyridine (0.204 g, 1.67 mmol) are added, and the mixture is cooled to 0° C. using an ice-water bath. Isobutyryl chloride (3.89 ml, 0.037 mol) is then added dropwise, and the mixture is stirred while warming to room temperature. The mixture is poured into water (100 ml), and the dichloromethane layer is separated, washed with saturated brine (100 ml), dried (MgSO4), treated with activated charcoal (300 mg), filtered and evaporated to give a pale pink solid.

WORKUP

后处理

  1. temperaturewhile warming to room temperature
  2. customthe dichloromethane layer is separated
  3. washwashed with saturated brine (100 ml)
  4. dry with materialdried (MgSO4)
  5. additiontreated with activated charcoal (300 mg)
  6. filtrationfiltered
  7. customevaporated
  8. customto give a pale pink solid