HRID1510417

反应详情

EQUATION

反应方程式

HRID 1510417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of sodium ethoxide (4.4 g, 64.6 mmol) in absolute ethanol (60 mL) was added 4-chloroacetophenone (5.0 g, 32.3 mmol) and the reaction mixture was stirred for five minutes at room temperature. Diethyl oxalate (7.0 mL, 51.7 mmol) in absolute ethanol (10 mL) was added and the reaction mixture was heated to reflux for 4 hours. After cooling to room temperature, acetic acid (7.0 mL) was added and the resulting light yellow solid was filtered, washed with ethanol and dried in vacuo to obtain ethyl 4-(4-chlorophenyl)-2,4-dioxobutanoate (8.3 g, 32.6 mmol).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 4 hours
  3. temperatureAfter cooling to room temperature
  4. filtrationthe resulting light yellow solid was filtered
  5. washwashed with ethanol
  6. customdried in vacuo