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
1.3 g (4.6 mmol) of 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)-2-pyrrolecarboxaldehyde and 50 ml of THF are introduced into a three-necked flask under a stream of nitrogen. 300 mg (10 mmol) of sodium hydride (80% in oil) are added portionwise and the mixture is stirred until the evolution of gas has ceased. 640 μl (10 mmol) of iodomethane are then added and the mixture is stirred at room temperature for one hour. The reaction medium is poured into water and extracted with ethyl acetate, and the organic phase is separated out after settling has taken place, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a column of silica eluted with a mixture of dichloromethane and heptane (70/30). After evaporation of the solvents, 600 mg (44%) of the expected product are collected.
WORKUP
后处理
- stirringthe mixture is stirred at room temperature for one hour
- extractionextracted with ethyl acetate
- customthe organic phase is separated out after settling
- dry with materialdried over magnesium sulphate
- customevaporated
- customThe residue obtained
- customis purified by chromatography on a column of silica
- washeluted with a mixture of dichloromethane and heptane (70/30)
- customAfter evaporation of the solvents, 600 mg (44%) of the expected product
- customare collected