HRID2420745

反应详情

EQUATION

反应方程式

HRID 2420745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 4.0 M hydrochloric acid in dioxane (1 mL) was added dropwise to a solution of amide 7 (204 mg, 0.43 mmol) in dichloromethane (3 mL) which had been pre-cooled to 0° C. The reaction was allowed to warm to ambient temperature, stirred for 2 hours, and the solvent then removed under vacuum. Recrystallization from methanol and diethyl ether produced salt 8 (123 mg, 84%) as a white solid: 1H NMR (300 MHz, CD3OD) δ 1.34 (s, 12H), 1.58-1.66 (m, 4H), 2.43 (t, 2H, J=7.4 Hz), 2.90 (t, 2H, J=7.5 Hz), 3.20-3.28 (m, 4H), 3.78-3.83 (m, 4H); m/z (ESI) 270 [C15H31N3O+H]+.

WORKUP

后处理

  1. temperatureto warm to ambient temperature
  2. customthe solvent then removed under vacuum
  3. customRecrystallization from methanol and diethyl ether produced salt 8 (123 mg, 84%) as a white solid