反应详情

In dichloromethane (40 ml), N-tert-butoxycarbonylpiperazine (2.00 g) was dissolved, followed by the addition of triethylamine (1.78 ml). To the resulting solution, methanesulfonyl chloride (0.91 ml) was added dropwise under ice cooling. After stirring for one hour under ice cooling, the reaction mixture was diluted with dichloromethane (20 ml), washed with a 5% aqueous citric acid solution, water and saturated aqueous NaCl solution and dried over anhydrous magnesium sulfate. The residue obtained by distilling off the solvent under reduced pressure was recrystallized from a mixed solvent of ethyl acetate and hexane, whereby the title compound (2.58 g, 91%) was obtained.

1. washwashed with a 5% aqueous citric acid solution, water and saturated aqueous NaCl solution
2. dry with materialdried over anhydrous magnesium sulfate
3. customThe residue obtained
4. distillationby distilling off the solvent under reduced pressure
5. customwas recrystallized from a mixed solvent of ethyl acetate and hexane, whereby the title compound (2.58 g, 91%)
6. customwas obtained