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
- 0 °C
PROCEDURE
实验过程
2.0 g of the monohydrate of 5-(4-{[6-(4-amino-3,5-dimethylphenoxy)-1-methyl-1-H-benzimidazol-2-yl]methoxy}benzyl)-1,3-thiazolidine-2,4-dione dihydrochloride obtained by a method similar to the method described in Example 1-1 was suspended in 100 ml of water. The resulting suspension was refluxed for 2 hours. The reaction mixture was cooled to 0° C. and agitated for 1 hour. The obtained crystalline form was filtered off and rinsed with water. The obtained moist crystalline form was dried for 14 hours at a pressure of approximately 80 kPa and at 50° C. to give a crystalline form, wherein the proportion of 5-(4-{[6-(4-amino-3,5-dimethylphenoxy)-1-methyl-1-H-benzimidazol-2-yl]methoxy}benzyl)-1,3-thiazolidine-2,4-dione and hydrochloric acid was approximately 1 to 1.1.
WORKUP
后处理
- temperatureThe resulting suspension was refluxed for 2 hours
- filtrationThe obtained crystalline form was filtered off
- washrinsed with water
- customThe obtained moist crystalline form was dried for 14 hours at a pressure of approximately 80 kPa and at 50° C.