HRID1651091

反应详情

EQUATION

反应方程式

HRID 1651091 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 145 g of [R-(R*,R*)]-alpha-hydroxy-N-[1-methyl-4-(3-pyridinyl)butyl]benzeneacetamide in 900 mL of 6N HCl was treated with 80 mL of conc. HCl and then was heated at reflux for 2 days. After most of the solvent was removed under reduced pressure, the residue was made decidedly basic with 10N NaOH in an argon atmosphere, and extracted with dichloromethane (1×1.2 L; 2×600 mL). The dried (K2CO3) extracts were evaporated and the crude product was distilled to give 78.5 g of (R)-alpha-methyl-3-pyridinebutanamine, (bp 95° C./0.2 mm).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 days
  3. customAfter most of the solvent was removed under reduced pressure
  4. extractionextracted with dichloromethane (1×1.2 L; 2×600 mL)
  5. dry with materialThe dried (K2CO3) extracts
  6. customwere evaporated
  7. distillationthe crude product was distilled