HRID1458562

反应详情

EQUATION

反应方程式

HRID 1458562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(cyanomethyl)methanesulphonamide (100 mg, 0.256 mmol) and tributyltin azide (170 mg, 0.512 mmol) (Synthesis, 1976, 329) in toluene (10 ml) was heated at reflux for 18 hours. After cooling the mixture was concentrated under reduced pressure and the residue purified by flash chromatography (gradient elution from dichloromethane to 90:10:1 dichloromethane: methanol:ammonia) to give N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(5-tetrazolylmethyl) methanesulphonamide as an off-white solid (78 mg, 70%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. temperatureAfter cooling the mixture
  4. concentrationwas concentrated under reduced pressure
  5. customthe residue purified by flash chromatography (gradient elution from dichloromethane to 90:10:1 dichloromethane: methanol:ammonia)