| 摘要 |
Busulfan drug intermediates 1, 4 - methyl sulfonic acid butyl ester synthesis method, comprising the following steps: the reaction vessel was added 0.15 mol 1,4-butanediol (2), 150-170ml triethylamine, the temperature of the solution is reduced to 3 - 5 0C, control the stirring speed 130-160rpm, slowly added 0.36-0.38mol methanesulfonic acid amine (3), after the completion of the dropwise addition, the solution temperature is raised to 35-40 0C, stirred for 3-4h, the temperature of the solution is reduced to 15 - 20 0C, the precipitated solid was filtered, washed with saline solution, dehydrated with dehydrating agent , recrystallized from cyclohexane solution, got white solid 1, 4 - methyl sulfonic acid butyl ester. |
