Reaktion #217606

Reaktionsgleichung

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

Lösungsmittel

pyridine dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigequenched with methanol
2. 2
   Einengenconcentrated in vacuo
3. 3
   Waschenwashed with methanol and 2M ammonia in methanol
4. 4
   EinengenThe combined basic fractions were concentrated in vacuo
5. 5
   Sonstigethe resulting residue was purified by column chromatography (FlashMaster) (gradient of dichloromethane to 4% metlianol:dichloromethane)

Vorschrift

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]+.

Quelle