HRID1375722

反应详情

EQUATION

反应方程式

HRID 1375722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl (2S)-3-[4-(3-{4-[(tert-butoxycarbonyl)amino]phenyl}propoxy)phenyl]-2-ethoxypropanoate (350 mg, 0.742 mmol) was dissolved in THF (10 ml). Under stirring, lithium hydroxide in water (5 ml) was added. The mixture was stirred at room temperature and followed by HPLC. After 4 hours, the reaction was stopped. More lithium hydroxide (9 mg) was added. The mixture was stirred overnight. It was then evaporated in vacuum to remove THF. The residue was extracted with diethyl ether and then acidified with 10% hydrochloric acid, pH˜3, and extracted with ethyl acetate (×2). The organic phases were combined and washed with brine and dried with magnesium sulfate. The solvent was evaporated and white solid product (315 mg) was left, yield 96%.

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature
  2. stirringThe mixture was stirred overnight
  3. customIt was then evaporated in vacuum
  4. customto remove THF
  5. extractionThe residue was extracted with diethyl ether
  6. extractionextracted with ethyl acetate (×2)
  7. washwashed with brine
  8. dry with materialdried with magnesium sulfate
  9. customThe solvent was evaporated
  10. waitwhite solid product (315 mg) was left