HRID50618

反应详情

EQUATION

反应方程式

HRID 50618 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The N-isopropyl-6-amino-1,2,3,4-tetrahydrocarbazole (9.84 g) and 5.05 g of triethylamine were dissolved in 100 mL of dichloromethane, and added dropwise with 7.85 g of phenyl chloroformate. The reaction mixture was stirred at room temperature for 3 hours, then washed with 10% aqueous citric acid and then with saturated aqueous sodium hydrogencarbonate, and dried over anhydrous sodium sulfate. After the solvent was evaporated under reduced pressure, the residue was purified by silica gel chromatography (eluent: hexane/ethyl acetate=8/2) and recrystallized from a mixture of hexane and ethyl acetate, to obtain 2.27 g of N-isopropyl-6-phenoxycarbonylamino-1,2,3,4-tetrahydrocarbazole.

WORKUP

后处理

  1. washwashed with 10% aqueous citric acid
  2. dry with materialwith saturated aqueous sodium hydrogencarbonate, and dried over anhydrous sodium sulfate
  3. customAfter the solvent was evaporated under reduced pressure
  4. customthe residue was purified by silica gel chromatography (eluent: hexane/ethyl acetate=8/2)
  5. customrecrystallized from a mixture of hexane and ethyl acetate