HRID1919148

反应详情

EQUATION

反应方程式

HRID 1919148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of ethyl 3-(2-aminoethyl)-3-azatricyclo[5.2.1.02,6]deca-2(6),4-diene-4-carboxylate (334e) (1.8 g, 7.2 mmol) in ethanol (40 mL) was added sodium meth-oxide (2.5 g, 36 mmol). The mixture was heated at 65° C. for 12 hours. It was then cooled to room temperature. The solvent was evaporated to dryness. The residue was purified by column chromatography eluting with 20:1 methylene chloride/methanol to give 334f as a brown solid (800 mg, 53%). MS: [M+H]+ 203.

WORKUP

后处理

  1. temperatureIt was then cooled to room temperature
  2. customThe solvent was evaporated to dryness
  3. customThe residue was purified by column chromatography
  4. washeluting with 20:1 methylene chloride/methanol