HRID389071

反应详情

EQUATION

反应方程式

HRID 389071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. custombrought to 80° C.
  2. temperatureThe mass was maintained
  3. customthe un-dissolved residue was removed by filtration
  4. temperaturemaintained at this temperature for 1 hour
  5. customThe obtained solid was separated by filtration
  6. customdried at 80° C. at atmospheric pressure for 10 hours in a nitrogen flow