HRID452602
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- washwashed with ethyl acetate
- extractionextracted with ethyl acetate/tetrahydrofuran
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure