HRID219626

反应详情

EQUATION

反应方程式

HRID 219626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of compound 7-((1S)-1-(4-bromophenyl)ethylamino)-2-methyl-4-phenylhept-1-en-4-ol (2.2 g, 5.5 mmol) in CH2Cl2 (50 mL) was added triphosgene (3.2 g, 11 mmol) and Et3N (1.7 g, 16.5 mmol) at 0° C. The mixture was stirred at room temperature overnight, and put at room temperature for 3 days, the volatile was evaporated. The resulting mixture was washed with 1 N aq HCl and extracted with CH2Cl2. The combined organic phase was dried over Na2SO4 and concentrated to give the crude final product, which was purified by chromatography to afford two isomers.

WORKUP

后处理

  1. waitput at room temperature for 3 days
  2. customthe volatile was evaporated
  3. washThe resulting mixture was washed with 1 N aq HCl
  4. extractionextracted with CH2Cl2
  5. dry with materialThe combined organic phase was dried over Na2SO4
  6. concentrationconcentrated