HRID37705
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 mixture consisting of 5-benzyloxytryptophol (7.0 g, 0.0262 mol), diethyl ketone (10 mL), benzene (400 mL) and p-toluene sulfonic acid is refluxed for 3.5 hours using a Dean-Stark tap to remove the water. The reaction mixture is cooled to room temperature, washed with 5% sodium bicarbonate, water (200 mL), brine (200 mL), dried (MgSO4), filtered and concentrated to give 9.9 g of crude product. The crude product is flash chromatographed on silica gel using 15% ethyl acetate/hexane as an eluent to afford 6.5 g of pure title compound.
WORKUP
后处理
- temperatureis refluxed for 3.5 hours
- customto remove the water
- washwashed with 5% sodium bicarbonate, water (200 mL), brine (200 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customto give 9.9 g of crude product
- customchromatographed on silica gel using 15% ethyl acetate/hexane as an eluent