HRID1625

反应详情

EQUATION

反应方程式

HRID 1625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto reflux for 6 hours
  2. washThe reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml)
  3. washThe combined aqueous layer was washed with diethyl ether (4×120 ml)
  4. washThe acidic solution was washed with ethyl acetate (3×200 ml)
  5. dry with materialthe combined organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness