HRID2301077
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 66 mg (1.65 mmol) portion of sodium hydride was added to 10 ml of DMF solution containing 300 mg (1.10 mmol) of 2-t-butoxycarbonyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole and stirred at room temperature for 30 minutes, and then 103 μl (1.65 mmol) of methyl iodide were added thereto and stirred overnight at room temperature. The reaction solution was extracted with ethyl acetate and washed with water. After drying (Na2SO4), the solvent was removed by evaporation under a reduced pressure and the resulting oil was purified by a silica gel column chromatography (60 cc; elution by ethyl acetate-hexane=1:5) to obtain 200 mg of the title compound (63% in yield).
WORKUP
后处理
- stirringstirred overnight at room temperature
- extractionThe reaction solution was extracted with ethyl acetate
- washwashed with water
- dry with materialAfter drying (Na2SO4)
- customthe solvent was removed by evaporation under a reduced pressure
- customthe resulting oil was purified by a silica gel column chromatography (60 cc; elution by ethyl acetate-hexane=1:5)