反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 27.5 °C
PROCEDURE
实验过程
Sunitinib (10 g) was suspended in methanol (1540 mL) under stirring and L-malic acid (3.36 g) was added to it at a temperature 25-30° C. The reaction mass was stirred to get a clear solution. It was filtered and methanol was distilled off under vacuum below 40° C. Acetonitrile (50 mL) was charged and the solvent was distilled off. It was cooled to 25-30° C. 380 mL of acetonitrile was added to the mass and it was mentained at 45-50° C. under stirring for a period of 15 minutes. The reaction mass was cooled to 30-35° C. The solid obtained was filtered and washed with acetonitrile (10 mL). The resultant compound was suck dried and dried under vacuum over a period of 4-5 hrs at 50° C. to obtain sunitinib L-malate. (12.0 g; yield 90%)
WORKUP
后处理
- stirringThe reaction mass was stirred
- customto get a clear solution
- filtrationIt was filtered
- distillationmethanol was distilled off under vacuum below 40° C
- additionAcetonitrile (50 mL) was charged
- distillationthe solvent was distilled off
- addition380 mL of acetonitrile was added to the mass and it
- customwas mentained at 45-50° C.
- stirringunder stirring for a period of 15 minutes
- temperatureThe reaction mass was cooled to 30-35° C
- customThe solid obtained
- filtrationwas filtered
- washwashed with acetonitrile (10 mL)
- customdried
- customdried under vacuum over a period of 4-5 hrs at 50° C.