HRID1166161
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
8-(2,6-dimethylbenzylamino)-2-hydroxymethyl-3-methylimidazo[1,2-a]pyridine (0.4 g, 1.3 mmol) and ethyl chloroformate (0.13 ml, 1.3 mmol) were solved in methylene chloride (20 ml) and were refluxed for 3 h. An additional amount of ethyl chloroformate (0.13 ml, 1.3 mmol) was added and the reaction mixture was refuxed 20 h. A sodium bicarbonate solution was added, the organic layer was separated dried (Na2SO4) and evaporated under reduced pressure. Purification of the residue by column chromatography on silica gel using diethyl ether as eluent and crystallization from diethyl ether: petroleum ether (1:2) gave 0.11 g (23%) of the title compound.
WORKUP
后处理
- temperaturewere refluxed for 3 h
- customthe organic layer was separated
- dry with materialdried (Na2SO4)
- customevaporated under reduced pressure
- customPurification of the residue by column chromatography on silica gel
- customcrystallization from diethyl ether: petroleum ether (1:2)