反应详情

Absolute piperazine (206 g) was dissolved in 500 ml of chloroform and 66.3 g of cinnamoyl chloride was added gradually at 0° C while mixing. The addition required 3 hours. After mixing was continued for another 2 hr., precipitates were filtered and then the filtrate (chloroform layer) was washed with 50 ml of 5% sodium hydroxide and 50 ml of water. The residues obtained after solvents were distilled away in vacuo were subjected to silica gel column chromatography (eluants were mixtures of chloroform and methanol). Thus crystalline N-cinnamoyl piperazine was obtained. Melting point of the product was 30°-40° C and the product was very hygroscopic. The yield was 30%.

1. additionwhile mixing
2. additionThe addition required 3 hours
3. additionAfter mixing
4. custom, precipitates
5. filtrationwere filtered
6. washthe filtrate (chloroform layer) was washed with 50 ml of 5% sodium hydroxide and 50 ml of water
7. customThe residues obtained after solvents
8. distillationwere distilled away in vacuo