反应详情

A solution of 3-(cis-3,5-dimethyl-1-piperazinyl)-4-(methyloxy)aniline (D2) (800 mg, 3.40 mmol) in dichloromethane (50 ml) was treated with morpholinomethyl-polystyrene HL resin (1.70 g, 4.0 mmol/g loading, 6.80 mmol) followed by 4-bromobenzenesulfonyl chloride (1.30 g, 5.09 mmol). The resulting solution was stirred at room temperature overnight and was then filtered, washing with methanol, and the filtrate concentrated in vacuo. The residue was then purified using an SCX ion exchange cartridge (Varian bond-elute) eluting with methanol followed by ammonia (2M in methanol). The appropriate fractions were combined and reduced in vacuo to afford a crude product which was purified further by chromatography on silica gel eluting with (0 to 20% methanol in dichloromethane) to afford the title compound (E101). MS (ES+) m/e 454/456 [M+H]+.

1. filtrationwas then filtered
2. washwashing with methanol
3. concentrationthe filtrate concentrated in vacuo
4. customThe residue was then purified
5. washan SCX ion exchange cartridge (Varian bond-elute)
6. washeluting with methanol
7. customto afford a crude product which
8. customwas purified further by chromatography on silica gel eluting with (0 to 20% methanol in dichloromethane)