HRID1770098

反应详情

EQUATION

反应方程式

HRID 1770098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Benzoyl-4-methyl isonipecotic acid (1.21 g, 4.88 mmol) was dissolved in 20 mL of 6N HCl and refluxed overnight. The mixture was cooled and benzoic acid removed by filtration. The filtrate was evaporated and crystallization from acetone/dichloromethane provided 0.62 g of 4-methyl isonipecotic acid (90%). 1H NMR (300 MHz DMSO d6) δ9.0 (s, 1H), 3.1 (m, 2H), 2.7 (m, 2H), 2.0 (m, 2 H), 1.6 (m, 2H), 1.1 (s, 3H).

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. temperatureThe mixture was cooled
  3. custombenzoic acid removed by filtration
  4. customThe filtrate was evaporated
  5. customcrystallization from acetone/dichloromethane