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
PROCEDURE
实验过程
One specific variant of this aspect of the invention involves dissolving magnesium at a temperature of 30° C. to 60° C. in a straight or branched lower alkanol (one to four carbons) solvent, adding haloalkane (one to three carbons) solvent, cooling to 0° C. to 15° C., adding esomeprazole base in a straight or branched lower alkanol solvent to generate a reaction mass, decomposing the reaction mass by pouring the mass into water and stirring for one to two hours, filtering out the resulting solid by conventional methods, suspending the solid obtained by filtering in a solvent such as acetone and stirring for one to two hours, filtering out the solid from the suspension by conventional methods (to remove excess magnesium), dissolving the solid resulting from the filtering in a straight or branched lower alkanol solvent and filtering the solution a straight or branched lower alkanol solvent, distilling off the solvent from the filtrate under reduced pressure, suspending the resulting solid in a solvent such as ethyl acetate (to crystallize solid), then either filtering by conventional methods; or adding esomeprazole magnesium in the form of an amorphous solid as seeding material and cooling to a temperature of 0° C. to 20° C. and then filtering by conventional methods, and drying the resulting solid at a temperature of 3° C. to 100° C., preferably 60° C., to obtain a hydrate of esomeprazole magnesium in the form of an amorphous solid.
WORKUP
后处理
- temperaturecooling to 0° C. to 15° C.
- filtrationfiltering out the resulting solid by conventional methods
- customobtained
- filtrationby filtering in a solvent such as acetone
- stirringstirring for one to two hours
- filtrationfiltering out the solid from the suspension by conventional methods (to remove excess magnesium)
- dissolutiondissolving the solid
- customresulting from the filtering in a straight or branched lower alkanol solvent
- filtrationfiltering the solution a straight or branched lower alkanol solvent
- distillationdistilling off the solvent from the filtrate under reduced pressure
- additionor adding esomeprazole magnesium in the form of an amorphous solid
- temperaturecooling to a temperature of 0° C. to 20° C.
- filtrationfiltering by conventional methods
- customdrying the resulting solid at a temperature of 3° C. to 100° C., preferably 60° C.