HRID1513318

反应详情

EQUATION

反应方程式

HRID 1513318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a 200 mL flask, dried oripavine (10.00 g, 95% wt/wt %) was dissolved in HOAc/H2O (1:4, 100 mL) and cooled to 5° C. to 10° C. Peroxyacetic acid, CH3CO3H, (9.1 mL, 32% wt/wt %) was added over 3 minutes and the reaction mixture was stirred at 5° C. to 10° C. for 30 minutes. HPLC data showed that the reaction was completed. The reaction mixture was allowed to warm to 25° C. for 30 minutes. H2C2O4 (3.0 g) was added to the reaction mixture, and was stirred at room temperature for 30 minutes and then heated to 50° C. for 30 minutes. The solution was assayed by HPLC and >99% conversion was observed.

WORKUP

后处理

  1. temperaturecooled to 5° C. to 10° C
  2. stirringwas stirred at room temperature for 30 minutes
  3. temperatureheated to 50° C. for 30 minutes