HRID1458562
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 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
- temperaturewas heated
- temperatureat reflux for 18 hours
- temperatureAfter cooling the mixture
- concentrationwas concentrated under reduced pressure
- customthe residue purified by flash chromatography (gradient elution from dichloromethane to 90:10:1 dichloromethane: methanol:ammonia)