HRID389071
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
- 15 °C
PROCEDURE
实验过程
A jacketed glass reactor was fed with 100 ml of water and brought to 80° C.; 0.8 g of argatroban monohydrate was added at this temperature. The mass was maintained under stirring for 10 minutes at this temperature then the un-dissolved residue was removed by filtration. The mother liquors were quickly cooled to 15° C. (in about 2 minutes) and maintained at this temperature for 1 hour. The obtained solid was separated by filtration and dried at 80° C. at atmospheric pressure for 10 hours in a nitrogen flow, giving 0.5 g of argatroban anhydrous (HPLC purity=99.9%; isomer ratio=60.6:39.4; KF=0.26%). Yield 65%.
WORKUP
后处理
- custombrought to 80° C.
- temperatureThe mass was maintained
- customthe un-dissolved residue was removed by filtration
- temperaturemaintained at this temperature for 1 hour
- customThe obtained solid was separated by filtration
- customdried at 80° C. at atmospheric pressure for 10 hours in a nitrogen flow