反应详情

温度

0 °C

A mixture of (R)-(1,4-dibenzylpiperazin-2-yl)methanol (4.00 g, 13.49 mmol, US2007/0088039) and Hünig's base (2.35 mL, 13.49 mmol) in CH2Cl2 (27 mL) was stirred at 0° C. and methanesulfonyl chloride (1.04 mL, 13.49 mmol) was added drop-wise. The reaction mixture was filtered through a short pad of silica gel, using 19:1 CH2Cl2/Et2O (1000 mL) to rinse. The filtrate was concentrated in vacuo while maintaining the temperature below 25° C. Diethyl ether was added to the residue, the resulting slurry was placed in a sonicator for 1 min, filtered through a fitted funnel and the filtrate was concentrated to give a white solid ((2R)-1,4-dibenzyl-2-piperazinyl)methyl methanesulfonate (4.42 g).

1. filtrationThe reaction mixture was filtered through a short pad of silica gel
2. washto rinse
3. concentrationThe filtrate was concentrated in vacuo
4. temperaturewhile maintaining the temperature below 25° C
5. additionDiethyl ether was added to the residue
6. filtrationfiltered through a fitted funnel
7. concentrationthe filtrate was concentrated