Sulfuric Acid → HCID 58522010, 화합물

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[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([CH3:13])[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1.S(=O)(=O)(O)O.[Br:19]N1C(=O)CCC1=O>>[Br:19][C:7]1[CH:6]=[C:5]([S:8]([N:11]([CH3:13])[CH3:12])(=[O:10])=[O:9])[CH:4]=[CH:3][C:2]=1[F:1]

참가 물질

반응물 3

HCID 1118Sulfuric Acid

HCID 67184N-bromobutanimide

HCID 7993014-fluoro-N,N-dimethylbenzenesulfonamide

생성물 1

HCID 58522010HCID 58522010, 화합물수율 82%

실험 절차

A solution of 4-fluoro-N,N-dimethylbenzenesulfonamide (1.80 g; 8.86 mmol) in conc. sulfuric acid (7 ml; 130 mmol) was treated with N-bromosuccinimide (1 730 mg; 9.74 mmol) and stirred at RT for 3 h. The reaction mixture was carefully poured on crushed ice, extracted with AcOEt and the organic phase was washed with a 0.1 N solution of NaOH in water twice, then with brine twice. The organic phase was dried on MgSO4, filtered and concentrated under reduced pressure to give the title compound as a white solid (2.04 g, 82%).

후처리

additionThe reaction mixture was carefully poured
customon crushed ice
extractionextracted with AcOEt
washthe organic phase was washed with a 0.1 N solution of NaOH in water twice
customThe organic phase was dried on MgSO4
filtrationfiltered
concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록: ord-7beaa1bc7d274309934cdfb3054616c8
출처 데이터셋: uspto-grants-2012_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08273769B2

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