HRID547116

反应详情

EQUATION

反应方程式

HRID 547116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (0.25 mL) was added to a solution of (S)-t-butoxycarbonylamino-[4′-(1-{4-[3-(t-butyl-dimethyl-silanyloxy)-4,4-dimethyl-pentyl]-3-methyl-phenyl}-1-ethyl-propyl)-2′-methyl-biphenyl-4-yl]acetic acid methyl ester (Example 166-(2); 20.3 mg, 0.0273 mmol) in dichloromethane (1.3 mL) at room temperature, and the mixture was stirred at room temperature for 30 minutes. The solvent in the reaction solution was distilled off under reduced pressure, and the residue was diluted with diethyl ether. The mixture was adjusted to pH 7 with aqueous sodium bicarbonate solution, followed by extraction with diethyl ether. The extract was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=2/1) to give the title compound (12.0 mg, 83%).

WORKUP

后处理

  1. distillationThe solvent in the reaction solution was distilled off under reduced pressure
  2. additionthe residue was diluted with diethyl ether
  3. extractionfollowed by extraction with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate=2/1)