HRID1500388

反应详情

EQUATION

反应方程式

HRID 1500388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe reaction mass was stirred
  2. customto get a clear solution
  3. filtrationIt was filtered
  4. distillationmethanol was distilled off under vacuum below 40° C
  5. additionAcetonitrile (50 mL) was charged
  6. distillationthe solvent was distilled off
  7. addition380 mL of acetonitrile was added to the mass and it
  8. customwas mentained at 45-50° C.
  9. stirringunder stirring for a period of 15 minutes
  10. temperatureThe reaction mass was cooled to 30-35° C
  11. customThe solid obtained
  12. filtrationwas filtered
  13. washwashed with acetonitrile (10 mL)
  14. customdried
  15. customdried under vacuum over a period of 4-5 hrs at 50° C.