반응 #685012

반응 방정식

NBS

Intermediate 2

2,2,2-Trifluoro-1-(4-(5-fluoro-2-methylphenylsulfonyl)piperazin-1-yl)ethanone

AIBN

→

title compound

수율 49.0%

1-(4-(2-(Bromomethyl)-5-fluorophenylsulfonyl)piperazin-1-yl)-2,2,2-trifluoroethanone

수율 49.0%

용매

CCl4

반응 조건

후처리

1. 1
   온도to reflux
2. 2
   온도the mixture was refluxed for 4 h
3. 3
   온도cooled
4. 4
   여과filtered
5. 5
   기타to remove solids
6. 6
   농축Concentration and purification by flash chromatography (0% to 25% EtOAc/hexane)

실험 절차

To a solution of Intermediate 2 (9.5 g, 27 mmol) in CCl4 (70 mL) was added AIBN (0.5 g, 3 mmol) and the mixture was brought to reflux. NBS (5.3 g, 30 mmol) was added and the mixture was refluxed for 4 h, cooled and filtered to remove solids. Concentration and purification by flash chromatography (0% to 25% EtOAc/hexane) gave the title compound as colorless oil (5.715 g, 49% yield). 1H NMR (300 MHz, CDCl3) δ: 7.65-7.60 (2H, m), 7.33-7.27 (1H, m), 4.83 (2H, s), 3.82-3.79 (2H, m), 3.74-3.71 (2H, m), 3.34-3.30 (4H, m). LCMS (M+H) calcd for C13H14BrF4N2O3S: 433.97; found: 435.11.

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