HRID1791050

反应详情

EQUATION

反应方程式

HRID 1791050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

0.046 ml (2 equivalents) of bromotrichloromethane is added to 50 mg (0.23 mmol) of methyl 3-oxo-2,3-dihydro-1-benzoxepin-7-carboxylate, prepared according to example 49, and 214 mg (0.92 mmol) of triphenylphosphine in suspension in 0.5 ml of acetonitrile, which is stirred beforehand at 0° C. for 2 hours. The reaction medium is protected from light and is again stirred at ambient temperature for 15 minutes. After the conventional treatments, purification on a column of silica gel (ethyl acetate/heptane 5/95) provides 48 mg (74%) of methyl 3-(dichloromethylene)-2,3-dihydro-1-benzoxepin-7-carboxylate in the form of a white solid; M.p.=119–121° C.

WORKUP

后处理

  1. customprepared
  2. stirringis again stirred at ambient temperature for 15 minutes
  3. customAfter the conventional treatments, purification on a column of silica gel (ethyl acetate/heptane 5/95)