反应详情

3,4-Dichlorophenylisocyanate (3.43 g) and tert-butyl piperazine-1-carboxylate (3.40 g) were stirred for 18 hours in chloroform (20 ml) at room temperature. Trisamine resin (1 g) was added and the mixture stirred for 3 hours, then filtered off. Trifluoroacetic acid (10 ml) was added to the filtrate and this mixture was stirred for two hours. The reaction mixture was concentrated in vacuo and the resulting oil separated between ethyl acetate (100 ml) and saturated aqueous sodium bicarbonate solution (100 ml). The ethyl acetate layer was separated, dried over magnesium sulphate, filtered then concentrated in vacuo to give the title compound (5.47 g).

1. filtrationfiltered off
2. additionTrifluoroacetic acid (10 ml) was added to the filtrate
3. stirringthis mixture was stirred for two hours
4. concentrationThe reaction mixture was concentrated in vacuo
5. customthe resulting oil separated between ethyl acetate (100 ml) and saturated aqueous sodium bicarbonate solution (100 ml)
6. customThe ethyl acetate layer was separated
7. dry with materialdried over magnesium sulphate
8. filtrationfiltered
9. concentrationthen concentrated in vacuo