HRID1625
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
PROCEDURE
实验过程
A solution of 4-phenoxybenzonitrile (9.87 g), dibutyltin oxide (3.88 g), and trimethylsilyl azide (33.5 ml) in anhydrous toluene (200 ml) was heated to reflux for 6 hours. The reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml). The combined aqueous layer was washed with diethyl ether (4×120 ml) then acidified to pH 6 with concentrated hydrochloric acid. The acidic solution was washed with ethyl acetate (3×200 ml) and the combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to dryness to give 5-(4-phenoxyphenyl)-1H-tetrazole as a white powder.
WORKUP
后处理
- temperatureto reflux for 6 hours
- washThe reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml)
- washThe combined aqueous layer was washed with diethyl ether (4×120 ml)
- washThe acidic solution was washed with ethyl acetate (3×200 ml)
- dry with materialthe combined organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- customevaporated to dryness