HRID2115184

反应详情

EQUATION

反应方程式

HRID 2115184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a 100 mL reactor was charged amorphous irinotecan acetate (2.0 g) and methanol (14 mL). The reaction mixture was heated to 50° C. 2N hydrochloric acid (6.2 wt %, about 1.7 mL) was added to adjust the pH level to less than 4 in order to dissolve the solid particles. Ethyl acetate (40 mL) was added slowly to the mixture. The mixture was cooled to 0˜10° C. and stirred at this temperature for 1 hour. The solid particles were filtered and washed with cooled ethyl acetate (6 mL). The wet cake was dried in vacuum to give 1.66 g of irinotecan hydrochloride trihydrate Form III.

WORKUP

后处理

  1. dissolutionto dissolve the solid particles
  2. temperatureThe mixture was cooled to 0˜10° C.
  3. filtrationThe solid particles were filtered
  4. washwashed with cooled ethyl acetate (6 mL)
  5. customThe wet cake was dried in vacuum