HRID1604586
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 6-hydroxymethyl-1,2,3,4-tetrahydroquinoline (314 mg) in methanol (4 ml) was dropwise added acetic anhydride (589 mg) under ice-cooling, and the mixture was stirred for 1 hour at the same temperature. The solvent was removed in vacuo, and ethyl acetate and saturated sodium bicarbonate solution was added to the residue. The organic layer was washed with water and brine, dried and concentrated in vacuo. The residue was purified by preparative thin-layer chromatography (n-hexane:ethyl acetate=1:2, V/V) to give 1-acetyl-6-hydroxymethyl-1,2,3,4-tetrahydroquinoline (227 mg) as powder.
WORKUP
后处理
- temperaturecooling
- customThe solvent was removed in vacuo, and ethyl acetate and saturated sodium bicarbonate solution
- additionwas added to the residue
- washThe organic layer was washed with water and brine
- customdried
- concentrationconcentrated in vacuo
- customThe residue was purified by preparative thin-layer chromatography (n-hexane:ethyl acetate=1:2, V/V)