HRID1443506

反应详情

EQUATION

反应方程式

HRID 1443506 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

The ethyl ester 158 (460 mg, 0.713 mmol) was dissolved in THF:MeOH:H2O (2:1:1, 100 mL) and LiOH (1M) (7.13 mL mg, 7.13 mmol) was added to the solution. The reaction was heated to 50° C. for 16 hrs. THF and MeOH was then removed by rotary evaporation and the remaining solution was acidified with 20 mL 10% citric acid (aq). The water phase was extracted with CHCl3 (3×50 mL) and the organic phase was washed with brine. The organic phase was dried with Na2SO4, filtered and concentrated by rotary evaporation. The product was obtained as a white solid (0.363 g, 82%), LRMS (M+H) 617.

WORKUP

后处理

  1. customTHF and MeOH was then removed by rotary evaporation
  2. extractionThe water phase was extracted with CHCl3 (3×50 mL)
  3. washthe organic phase was washed with brine
  4. dry with materialThe organic phase was dried with Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation