反应详情

A solution of 5-(cis-3,5-dimethyl-1-piperazinyl)-2-chloroaniline (D34) (108 mg, 0.45 mmol) in pyridine:dichloromethane (1:1, 4 ml) was treated with 4-bromobenzenesulfonyl chloride (138 mg, 0.54 mmol). The solution was stirred at room temperature for 2 hours, quenched with methanol and concentrated in vacuo. The residue was applied to a SCX cartridge (Varian bond-elute, 5 g) and washed with methanol and 2M ammonia in methanol. The combined basic fractions were concentrated in vacuo and the resulting residue was purified by column chromatography (FlashMaster) (dichloromethane to 5% methanol:dichloromethane) to afford some pure product. The impure fractions were purified further by MDAP, and combined with the above pure product to afford the title product (D35). MS (ES+) m/e 458/460/462 [M+H]+.

1. customquenched with methanol
2. concentrationconcentrated in vacuo
3. washwashed with methanol and 2M ammonia in methanol
4. concentrationThe combined basic fractions were concentrated in vacuo
5. customthe resulting residue was purified by column chromatography (FlashMaster) (dichloromethane to 5% methanol:dichloromethane)
6. customto afford some pure product
7. customThe impure fractions were purified further by MDAP