HRID1154329
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 solution of 2.24 g. of furoic acid, 3.24 g. of N,N'-carbonyldiimidazole and 80 ml. of tetrahydrofuran was allowed to stir at room temperature for 2 hours. A 4.0 g. portion of 1H-imidazole-1-propanamine dihydrochloride was added and the mixture was stirred at room temperature overnight. The mixture was then heated for 5 hours, 5 ml. of water was added, heating resumed for 30 minutes and then the mixture was concentrated to remove most of the solvent. Dichloromethane and 60 ml. of 1N sodium hydroxide were added, the organic layer was separated, washed twice with water, dried and concentrated, giving 2.0 g. of the desired product, m.p. 127°-129° C.
WORKUP
后处理
- stirringthe mixture was stirred at room temperature overnight
- temperatureThe mixture was then heated for 5 hours
- temperatureheating
- waitresumed for 30 minutes
- concentrationthe mixture was concentrated
- customto remove most of the solvent
- additionof 1N sodium hydroxide were added
- customthe organic layer was separated
- washwashed twice with water
- customdried
- concentrationconcentrated
- customgiving 2.0 g