반응 #1869163

반응 방정식

cytarabine

HCl

→

cytarabine hydrochloride

수율 96.3%

용매

methanol

methanol

반응 조건

후처리

1. 1
   기타A 5 L, 3-neck flask equipped with an overhead stirrer
2. 2
   기타HCl gas was bubbled in,
3. 3
   기타giving a very thick mixture
4. 4
   기타to 25° C
5. 5
   workup.STIRRINGThe mixture was stirred for 4 hours at 20° C.
6. 6
   여과then filtered
7. 7
   기타to collect the solid
8. 8
   세척The solid was washed with MTBE (3×250 mL)
9. 9
   기타dried in a vacuum oven at 70° C.

실험 절차

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.

출처