HRID974964

反应详情

EQUATION

反应方程式

HRID 974964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-benzyl-4-(2-cyano-2,2-diphenylethyl)piperidine (7.57 g, 19.9 mmol) (Example 23) in 90% sulphuric acid (45 ml) was heated at 100° C. for one hour, allowed to cool to room temperature, poured into ice, basified with saturated aqueous sodium carbonate solution and extracted into dichloromethane. The combined organic extracts were dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-10% methanol as eluant. Appropriate fractions were combined and evaporated to give the title compound (1.06 g, 13%) as a colourless foam which was characterised as a hemihydrate.

WORKUP

后处理

  1. additionpoured into ice
  2. extractionextracted into dichloromethane
  3. dry with materialThe combined organic extracts were dried over magnesium sulphate
  4. customevaporated
  5. customThe residue was purified by chromatography on silica
  6. customevaporated