HRID1173087

反应详情

EQUATION

反应方程式

HRID 1173087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 l (1 mol) of a tetrahydrofuran solution containing 1.0 M vinylmagnesium bromide was added to a tetrahydrofuran solution (300 ml) containing 65.0 g (301 mmol) of 2-bromo-5-methylnitrobenzene at −60° C. under stirring for one hour in nitrogen atmosphere. An aqueous saturated ammonium chloride and ethyl acetate were added to the reaction mixture solution, and the insoluble matters were filtered off. The filtrate was dried over magnesium sulfate and concentrated. Then, the residue was purified by silica gel column chromatography, to give 35.5 g of the title compound.

WORKUP

后处理

  1. filtrationthe insoluble matters were filtered off
  2. dry with materialThe filtrate was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThen, the residue was purified by silica gel column chromatography