反应 #217606

反应方程式

5-(cis-3,5-Dimethyl-1-piperazinyl)-2-chloroaniline

5-bromo-2-thiophenesulfonyl chloride

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title product

5-Bromo-N-[2-chloro-5-(cis-3,5-dimethyl-1-piperazinyl)phenyl]-2-thiophenesulfonamide

溶剂

pyridine dichloromethane

反应条件

后处理

1. 1
   其他quenched with methanol
2. 2
   浓缩concentrated in vacuo
3. 3
   洗涤washed with methanol and 2M ammonia in methanol
4. 4
   浓缩The combined basic fractions were concentrated in vacuo
5. 5
   其他the resulting residue was purified by column chromatography (FlashMaster) (gradient of dichloromethane to 4% metlianol:dichloromethane)

实验过程

A solution of 5-(cis-3,5-Dimethyl-1-piperazinyl)-2-chloroaniline (D34) (100 mg, 0.42 mmol) in pyridine:dichloromethane (1:1, 4 ml) was treated with 5-bromo-2-thiophenesulfonyl chloride (132 mg, 0.51 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) (gradient of dichloromethane to 4% metlianol:dichloromethane) to afford the title product (D36). MS (ES+) m/e 464/466/468 [M+H]+.

来源