反应详情

A solution of 5-(cis-3,5-dimethyl-1-piperazinyl)-2-(methyloxy)aniline (D4) (1.00 g, 4.25 mmol) in dichloromethane (50 ml) was treated with morpholinomethyl-polystyrene HL resin (2.10 g, 4.0 mmol/g loading, 8.50 mmol) followed by 5-bromo-2-thiophenesulfonyl chloride (1.33 g, 5.09 mmol). The resulting solution was stirred at room temperature overnight and was then filtered and the solvent evaporated. The residue was then chromatographed over silica gel (Flashmaster (II)) eluting with 0 to 10% methanol in dichloromethane 90% for 5 mins, 0-10% 20 mins and 10% 10 mins). The compound was then purified by mass directed autoprep HPLC and the residue further purified by SCX, eluting with methanol first and then NH4OH/methanol. (E122). MS (ES+) m/e 460/462 [M+H]+.

1. filtrationwas then filtered
2. customthe solvent evaporated
3. customThe residue was then chromatographed over silica gel (Flashmaster (II))
4. washeluting with 0 to 10% methanol in dichloromethane 90% for 5 mins
5. custom0-10% 20 mins and 10% 10 mins
6. customThe compound was then purified by mass
7. customthe residue further purified by SCX
8. washeluting with methanol first