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
To a solution of N-methylpyrrole (8.10 g, 0.1 mol) in ether (50 ml) was added a solution of chloral (16.21 g, 0.1 mol) in ether (50 ml). To this were added p-toluene-sulfonic acid (200 mg) and hydroquinone (5 mg). Then the mixture was refluxed for 15 hours. After adding triethylamine (5 ml), the mixture was stirred for 5 minutes. Brine (100 ml) was added and the organic layer separated. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were washed with brine (100 ml). After drying over magnesium sulfate, the organic solution was filtered through a bed of activated charcoal, and concentration afforded the adduct 1-methyl-2-(2',2',2'-trichloro-1'-hydroxyethyl)pyrrole (24.1 g) as pale brown prisms.
WORKUP
后处理
- temperatureThen the mixture was refluxed for 15 hours
- customthe organic layer separated
- extractionThe aqueous layer was extracted with ethyl acetate
- washthe combined organic layers were washed with brine (100 ml)
- dry with materialAfter drying over magnesium sulfate
- filtrationthe organic solution was filtered through a bed of activated charcoal, and concentration