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
The 2-t-butoxycarbonyl-9-carboxymethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole (1.65 g, 5.0 mmol) obtained in the above step (1) was dissolved in methylene chloride (30 ml), and the solution was mixed with carbonyldiimidazole (0.81 g, 5.0 mmol), stirred at room temperature for 30 minutes, mixed with 2 M dimethylamine-THF solution (3 ml, 6.0 mmol) and further subjected to 1 hour of the reaction. The reaction solution was concentrated, the resulting residue was dissolved in ethyl acetate (50 ml), washed with water and dried with anhydrous sodium sulfate, and then the solvent was removed by evaporation under a reduced pressure. By adding diisopropyl ether (30 ml) to the resulting residue, 1.71 g of the thus precipitated title compound (4.8 mmol, 96% in yield) was obtained as crystals.
WORKUP
后处理
- customfurther subjected to 1 hour of the reaction
- concentrationThe reaction solution was concentrated
- dissolutionthe resulting residue was dissolved in ethyl acetate (50 ml)
- washwashed with water
- dry with materialdried with anhydrous sodium sulfate
- customthe solvent was removed by evaporation under a reduced pressure
- additionBy adding diisopropyl ether (30 ml) to the resulting residue, 1.71 g of the