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
Methanol (100 ml) and sodium hydroxide solution (1 N, 22 mmol) were added to 2-t-butoxycarbonyl-9-methoxycarbonylmethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole (7.42 g, 21.5 mmol) and stirred at room temperature for 2 hours, the solvent was removed by evaporation under a reduced pressure, the thus obtained oily material was dissolved in ethyl acetate (100 ml) and then the ethyl acetate layer was washed with water, dried with anhydrous sodium sulfate and concentrated under a reduced pressure. The resulting residue was precipitated by adding diisopropyl ether (30 ml), thereby obtaining 5.29 g (16.0 mmol, 74.4% in yield) of 2-t-butoxycarbonyl-9-carboxymethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole.
WORKUP
后处理
- customthe solvent was removed by evaporation under a reduced pressure
- dissolutionthe thus obtained oily material was dissolved in ethyl acetate (100 ml)
- washthe ethyl acetate layer was washed with water
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated under a reduced pressure
- customThe resulting residue was precipitated
- additionby adding diisopropyl ether (30 ml)