반응 #217606

반응 방정식

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

5-bromo-2-thiophenesulfonyl chloride

→

title product

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

용매

pyridine dichloromethane

반응 조건

후처리

1. 1
   기타quenched with methanol
2. 2
   농축concentrated in vacuo
3. 3
   세척washed with methanol and 2M ammonia in methanol
4. 4
   농축The combined basic fractions were concentrated in vacuo
5. 5
   기타the resulting residue was purified by column chromatography (FlashMaster) (gradient of dichloromethane to 4% metlianol:dichloromethane)

실험 절차

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]+.

출처