HRID651989
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
1 g of 2-(2-methoxy-4-hydroxy-phenyl)-5H-imidazo[4,5-c]pyridin-4-one was suspended in 30 ml of sulfolane, 1.41 g of potassium carbonate were added, and the mixture was stirred at room temperature. After 15 minutes and again after one hour, 0.9 ml of propargyl bromide was added, and the mixture was then stirred for another 1.25 hours. The solvent was substantially evaporated in vacuo, and the residue was stirred with methylene chloride. After the precipitate had been filtered off and washed with water, the product contained in the organic phase was purified on a silica gel column (eluant: methylene chloride/ethanol 1:0 to 1:0.03). The product crystallized with half a mol of ethanol.
WORKUP
后处理
- waitagain after one hour
- stirringthe mixture was then stirred for another 1.25 hours
- customThe solvent was substantially evaporated in vacuo
- stirringthe residue was stirred with methylene chloride
- filtrationAfter the precipitate had been filtered off
- washwashed with water
- customwas purified on a silica gel column (eluant: methylene chloride/ethanol 1:0 to 1:0.03)
- customThe product crystallized with half a mol of ethanol