HRID2073495

反应详情

EQUATION

反应方程式

HRID 2073495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

33.1 g (53.8 mmol) of 1-[4,4-bis(4-fluorophenyl)butyl]-4-tritylpiperazine-2-carboxamide were dissolved in 180 ml of glacial acetic acid, 180 ml of water were added dropwise in the course of 15 minutes, the mixture was subsequently stirred for 90 minutes, the oily precipitate was decanted, 720 ml of H2O and a Little Celite®, a product from Johns-Mannville Corporation, New York, were added, the mixture was filtered and the filtrate was brought to pH 10 with concentrated NaOH and extracted with methylene chloride. The organic phase was dried and concentrated in vacuo.

WORKUP

后处理

  1. customthe oily precipitate was decanted
  2. addition720 ml of H2O and a Little Celite®, a product from Johns-Mannville Corporation, New York, were added
  3. filtrationthe mixture was filtered
  4. extractionextracted with methylene chloride
  5. customThe organic phase was dried
  6. concentrationconcentrated in vacuo