HRID452602

反应详情

EQUATION

反应方程式

HRID 452602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2,3-dihydro-1-benzofuran-5-carbonitrile (1.29 g, 8.89 mmol), sodium azide (1.16 g, 17.78 mmol), zinc bromide (1.00 g, 4.45 mmol), 2-propanol (15 mL) and water (30 mL) was stirred at 80° C. for 48 hr. The reaction mixture was basified with an aqueous sodium hydroxide solution, and washed with ethyl acetate. The aqueous layer was acidified with hydrochloric acid, and extracted with ethyl acetate/tetrahydrofuran. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give the title compound (1.10 g, yield 66%) as colorless crystals.

WORKUP

后处理

  1. washwashed with ethyl acetate
  2. extractionextracted with ethyl acetate/tetrahydrofuran
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure