反应详情

Pyridine (0.28 ml) was added to a stirred solution of 2-isopropylaniline (98 mg) and 3-(4-trichloroacetylpiperazin-1-yl)-4-methoxybenzenesulfonyl chloride (D4) (300 mg) in dichloromethane (4 ml) at room temperature. After 18 h the solution was washed with 1M hydrochloric acid (5 ml) then water (5 ml). The organic phase was stirred vigourously with 20% aq. potassium hydroxide (0.5 ml) for 18 h. A 10% aqueous solution of KH2PO4 (8 ml) was then added to the mixture and after 0.25 h stirring the layers were separated. The organic layer was dried (Na2SO4), acidified with 1M ethereal hydrogen chloride (2 ml) and concentrated to an oil which was stirred with acetone/diethyl ether to afford the title compound (E79) as a white solid (0.224 g, 83%). MH+ 390.

1. washAfter 18 h the solution was washed with 1M hydrochloric acid (5 ml)
2. additionA 10% aqueous solution of KH2PO4 (8 ml) was then added to the mixture and after 0.25 h
3. stirringstirring the layers
4. customwere separated
5. dry with materialThe organic layer was dried (Na2SO4)
6. concentrationconcentrated to an oil which
7. stirringwas stirred with acetone/diethyl ether