HRID2167689

反应详情

EQUATION

反应方程式

HRID 2167689 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a chloroform (20 mL) solution of methyl 3-(4-chlorophenyl)-3-oxopropanoate (1.0 g), bromine (0.12 mL) was added, and the resultant was stirred at 70° C. for 1 hour under sealed conditions. Then, bromine (0.12 mL) was further added thereto, and the resultant was further stirred at 70° C. for 1 hour under sealed conditions. The reaction solution was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (OH-type silica gel; hexane/ethyl acetate-gradient elution=100/0→75/25) to obtain the title compound (0.44 g) as a pale yellow oil.

WORKUP

后处理

  1. stirringthe resultant was further stirred at 70° C. for 1 hour under sealed conditions
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. customThe obtained residue was purified by silica gel column chromatography (OH-type silica gel; hexane/ethyl acetate-gradient elution=100/0→75/25)