HRID1500393

反应详情

EQUATION

反应方程式

HRID 1500393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

Sunitinib (1.0 g) was suspended in methanol (152 mL), followed by addition of sinapic acid (0.56 g) at 25-35° C. over a period of 15 minutes. After the stipulated time period, methanol was completely distilled off under vacuum below 45° C. The residue was treated with acetonitrile (38 mL) and refluxed. The reaction mass was maintained at reflux temperature for 60 minutes. The reaction mass was cooled to 25-35° C. for crystallization. The solid obtained was filtered, washed with acetonitrile, suck dried and dried under vacuum at 60° C. over 4-5 hr period to obtain sunitinib sinapinate.(1.3 g; yield:83%)

WORKUP

后处理

  1. distillationAfter the stipulated time period, methanol was completely distilled off under vacuum below 45° C
  2. additionThe residue was treated with acetonitrile (38 mL)
  3. temperaturerefluxed
  4. temperatureThe reaction mass was maintained
  5. temperatureat reflux temperature for 60 minutes
  6. customThe solid obtained
  7. filtrationwas filtered
  8. washwashed with acetonitrile, suck
  9. customdried
  10. customdried under vacuum at 60° C. over 4-5 hr period