HRID216290

反应详情

EQUATION

反应方程式

HRID 216290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A solution of the product of Example 274B (1.3 g) in tetrahydrofuran:water (25 mL, 4:1) was treated with triphenylphosphine (1.4 g, 2 equivalents), stirred at 70° C. for 2 hours and concentrated. The residue was partitioned between 1N HCl and dichloromethane. The aqueous layer was separated and made basic using 1N NaOH, extracted with dichloromethane and the organic extract was concentrated. The residue was purified by HPLC reverse phase chromatography using water (0.1% trifluoroacetic acid):acetonitrile (95:5) to acetonitrile (100%) to give 0.76 g (62%) of the title compound.

WORKUP

后处理

  1. concentrationconcentrated
  2. customThe residue was partitioned between 1N HCl and dichloromethane
  3. customThe aqueous layer was separated
  4. extractionextracted with dichloromethane
  5. extractionthe organic extract
  6. concentrationwas concentrated
  7. customThe residue was purified by HPLC reverse phase chromatography