تفاعل #217606

معادلة التفاعل

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

المذيبات

pyridine dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىquenched with methanol
2. 2
   تركيزconcentrated in vacuo
3. 3
   غسيلwashed with methanol and 2M ammonia in methanol
4. 4
   تركيزThe combined basic fractions were concentrated in vacuo
5. 5
   أخرىthe resulting residue was purified by column chromatography (FlashMaster) (gradient of dichloromethane to 4% metlianol:dichloromethane)

الإجراء التجريبي

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]+.

المصدر