HRID1500393
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- distillationAfter the stipulated time period, methanol was completely distilled off under vacuum below 45° C
- additionThe residue was treated with acetonitrile (38 mL)
- temperaturerefluxed
- temperatureThe reaction mass was maintained
- temperatureat reflux temperature for 60 minutes
- customThe solid obtained
- filtrationwas filtered
- washwashed with acetonitrile, suck
- customdried
- customdried under vacuum at 60° C. over 4-5 hr period