反应 #1869163

反应方程式

cytarabine

HCl

→

cytarabine hydrochloride

收率 96.3%

溶剂

methanol

methanol

反应条件

后处理

1. 1
   其他A 5 L, 3-neck flask equipped with an overhead stirrer
2. 2
   其他HCl gas was bubbled in,
3. 3
   其他giving a very thick mixture
4. 4
   其他to 25° C
5. 5
   workup.STIRRINGThe mixture was stirred for 4 hours at 20° C.
6. 6
   过滤then filtered
7. 7
   其他to collect the solid
8. 8
   洗涤The solid was washed with MTBE (3×250 mL)
9. 9
   其他dried in a vacuum oven at 70° C.

实验过程

A 5 L, 3-neck flask equipped with an overhead stirrer and thermocouple was charged with cytarabine (500 g, 2.06 mol) and methanol (2.0 L). The suspension was cooled to 2° C. HCl gas was bubbled in, giving a very thick mixture and an exotherm to 25° C. The suspension was diluted with methanol (0.5 L) to facilitate stirring. A total of 108 g (2.96 mol) of HCl gas was added. The mixture was stirred for 4 hours at 20° C. then filtered to collect the solid. The solid was washed with MTBE (3×250 mL) and dried in a vacuum oven at 70° C. to give 555 g (96% yield) of cytarabine hydrochloride as a flocculent, white solid.

来源