HRID1443506
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
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
- customTHF and MeOH was then removed by rotary evaporation
- extractionThe water phase was extracted with CHCl3 (3×50 mL)
- washthe organic phase was washed with brine
- dry with materialThe organic phase was dried with Na2SO4
- filtrationfiltered
- concentrationconcentrated by rotary evaporation