Réaction #1869163

Équation de réaction

cytarabine

HCl

→

cytarabine hydrochloride

Rendement 96.3%

Solvants

methanol

methanol

Conditions de réaction

Traitement

1. 1
   AutreA 5 L, 3-neck flask equipped with an overhead stirrer
2. 2
   AutreHCl gas was bubbled in,
3. 3
   Autregiving a very thick mixture
4. 4
   Autreto 25° C
5. 5
   workup.STIRRINGThe mixture was stirred for 4 hours at 20° C.
6. 6
   Filtrationthen filtered
7. 7
   Autreto collect the solid
8. 8
   LavageThe solid was washed with MTBE (3×250 mL)
9. 9
   Autredried in a vacuum oven at 70° C.

Mode opératoire

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.

Source