HRID1493414

反应详情

EQUATION

反应方程式

HRID 1493414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A mixture of 15.0 g (70.0 mmol) of 2,4-dihydroxybenzophenone, 10.7 g (70 mmol) of methyl bromoacetate, 19.3 g (0.14 mol) of potassium carbonate, and 125 ml of N,N-dimethylformamide is stirred at 25° C. for 18 hours. The reaction mixture is partitioned between diethyl ether and 0.5 N hydrochloric acid. Solids are removed by filtration, and the filtrate is dried over magnesium sulfate and concentrated. The concentrate is partially dissolved in diethyl ether, and solids are removed by filtration. The solid material is recrystallized from dichloromethane: 2-propanol to afford 13.7 g (69% yield) of the title compound, a pale yellow solid, mp 131°-4° C.

WORKUP

后处理

  1. customThe reaction mixture is partitioned between diethyl ether and 0.5 N hydrochloric acid
  2. customSolids are removed by filtration
  3. dry with materialthe filtrate is dried over magnesium sulfate
  4. concentrationconcentrated
  5. dissolutionThe concentrate is partially dissolved in diethyl ether
  6. customsolids are removed by filtration
  7. customThe solid material is recrystallized from dichloromethane