反应详情

A mixture of 1-methylpiperazine (5 ml.), N,N-dioctadecylcarbamylchloride (5.0 g.) and benzene (50 ml.) is refluxed and stirred for three hours. The white precipitate of 1-methylpiperazine hydrochloride is removed by filtration and the filtrate concentrated in vacuo to a yellow oil (4.5 g.). The oil is then charged on a silica gel pad and eluted with benzene in 50 ml. fractions. Fractions 10-15 are combined, a large volume of methanol added and the white crystalline material which separates filtered and dried, m.p. 46°-47° C. (1.45 g.).

1. temperatureis refluxed
2. customThe white precipitate of 1-methylpiperazine hydrochloride is removed by filtration
3. concentrationthe filtrate concentrated in vacuo to a yellow oil (4.5 g.)
4. additionThe oil is then charged on a silica gel pad
5. washeluted with benzene in 50 ml
6. additiona large volume of methanol added
7. filtrationthe white crystalline material which separates filtered
8. customdried