HRID1272585

反应详情

EQUATION

反应方程式

HRID 1272585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 30 g of ester E)-(S)-7-[3-(4-Fluoro-phenyl)-1-isopropyl-1H-indol-2-yl]-5-hydroxy-3-oxo-hept-6-enoic acid tert-butyl ester in 150 ml of ethanol is added under stirring 63 ml of sodium hydroxide solution while maintaining the temperature below 12° C. The solution is stirred for 1 hour, the mixture is concentrated at 25 mm Hg and 45° C., then 220 ml of water are added, destination is continued to a remaining volume of 100 ml , then 280 ml of water are added and the solution is washed with a total of 450 ml of MTBE in 3 portions. The aquous layer is concentrated at 25 mm Hg and 45° C. to a volume of about 200 ml, 150 ml water are added, and the clear aquous solution is lyophylized over 3 days. MS: 433.21

WORKUP

后处理

  1. temperaturewhile maintaining the temperature below 12° C
  2. concentrationthe mixture is concentrated at 25 mm Hg and 45° C.
  3. addition220 ml of water are added
  4. addition280 ml of water are added
  5. washthe solution is washed with a total of 450 ml of MTBE in 3 portions
  6. concentrationThe aquous layer is concentrated at 25 mm Hg and 45° C. to a volume of about 200 ml, 150 ml water
  7. additionare added
  8. waitthe clear aquous solution is lyophylized over 3 days