HRID878794

反应详情

EQUATION

反应方程式

HRID 878794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A suspension of rpm335 (0.155 g, 0.3734 mmol) in methanol (1 mL) and NaOH 1M (1 ml) was heated in the microwave at 150° C. for 5 min. The reaction mixture was cooled to 0° C., and the solvent distilled under reduced pressure and HCl (aq 4M, 5 ml) added. The orange precipitate was collected by filtration, washed with water (10 ml) and dried, to give pure rpm336 (0.139 g, 0.346 mmol, 92%). MS (API-ES): m/z 402 (M+H)+; HRMS (API-ES) m/z Found: 402.1116 (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. distillationthe solvent distilled under reduced pressure and HCl (aq 4M, 5 ml)
  3. additionadded
  4. filtrationThe orange precipitate was collected by filtration
  5. washwashed with water (10 ml)
  6. customdried
  7. customto give pure rpm336 (0.139 g, 0.346 mmol, 92%)