HRID258146

反应详情

EQUATION

反应方程式

HRID 258146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a 0° C. solution of 1,2,3,3a,8,8a-hexahydro-α-oxo-1,3a,8-trimethyl-5-pyrrolo[2,3-b]indole acetic acid, ethyl ester (0.25 g) in 95% ethanol (1.0 ml) was added a solution of 0.14 g of KOH in water (1.0 ml). The mixture was stirred at 0° C. for 30 minutes and then refluxed for 4 hours. The solution was cooled, the ethanol was removed under reduced pressure and the remaining aqueous residue was diluted with water (3.0 ml), cooled to 0° C. and neutralized with a 1.0N aqueous HCl solution. The water was then removed and the residue was taken up in dichloromethane and washed with water to remove any unreacted starting material. The aqueous washes were then concentrated to afford 1,2,3,3a,8,8a-hexahydro-α-oxo-1,3a,8-trimethyl-5-pyrrolo[2,3-b]indole acetic acid as a solid.

WORKUP

后处理

  1. temperaturerefluxed for 4 hours
  2. temperatureThe solution was cooled
  3. customthe ethanol was removed under reduced pressure
  4. additionthe remaining aqueous residue was diluted with water (3.0 ml)
  5. temperaturecooled to 0° C.
  6. customThe water was then removed
  7. washwashed with water
  8. customto remove
  9. concentrationThe aqueous washes were then concentrated