HRID1044721
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
- 70 °C
PROCEDURE
实验过程
Lapatinib ditosylate (3 g, 3.25 mmol, 99.3% HPLC purity was dissolved in DMF (18 mL) at 80° C. and stirred for 1 hour. The mixture was hot-filtered. MeCN (18 mL) was added into the filtrate at 80° C. The temperature was cooled to 70° C. and crystal precipitated. The mixture was kept at 70° C. for 1 h and then 60° C. for 1 h. The mixture was further cooled to 0° C. and stirred for 2 h. The crystals of lapatinib ditosylate were isolated by filtration and were dried at 40° C. under vacuum overnight. Lapatinib ditosylate (2.5 g, 2.70 mmol, 83% yield) with 99.9% HPLC purity was obtained. XRPD analysis (FIG. 9) indicated that this was Form 2 as disclosed in WO 2009/079541 A1.
WORKUP
后处理
- filtrationThe mixture was hot-filtered
- additionMeCN (18 mL) was added into the filtrate at 80° C
- customcrystal precipitated
- waitThe mixture was kept at 70° C. for 1 h
- wait60° C. for 1 h
- temperatureThe mixture was further cooled to 0° C.
- stirringstirred for 2 h