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5-Bromo-6-chloropyridine-3-sulfonyl chloride → 5-bromo-6-chloro-N-[2-(2,4-dichlorophenoxy)phenyl]pyridine-3-sulfonamide

HRID 746751
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HRID 746751 반응식
Cl.[Cl:2][C:3]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:4]=1[O:5][C:6]1[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=1[NH2:8].[Br:18][C:19]1[CH:20]=[C:21]([S:26](Cl)(=[O:28])=[O:27])[CH:22]=[N:23][C:24]=1[Cl:25]>N1C=CC=CC=1.C(OCC)(=O)C.Cl>[Br:18][C:19]1[CH:20]=[C:21]([S:26]([NH:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][C:4]2[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:3]=2[Cl:2])(=[O:28])=[O:27])[CH:22]=[N:23][C:24]=1[Cl:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 27936265-Bromo-6-chloropyridine-3-sulfonyl chlorideHCID 2795482Benzenamine, 4-(2,4-dichlorophenoxy)-, hydrochloride

생성물 1

HCID 38564715-bromo-6-chloro-N-[2-(2,4-dichlorophenoxy)phenyl]pyridine-3-sulfonamide

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 1049Pyridine용매
HCID 8857
Ethyl Acetate
용매

실험 절차

2-(2,4-Dichlorophenoxy)aniline HCl (1.14 g, 3.94 mmol) and 5-bromo-6-chloropyridine-3-sulfonyl chloride (1.26 g, 4.33 mmol) were dissolved in pyridine (4 mL) and allowed to stir at ambient temperature for 1 hour. The reaction mixture was then diluted with 100 mL of ethyl acetate, 80 mL of 0.5 M HCl. The organic layer was washed successively with 100 mL of 0.5 M HCl, twice with 100 mL of water, 100 mL of half-saturated brine and finally 100 mL of brine. Drying of the organic layer over sodium sulfate was followed by filtration and solvent removal under reduced pressure. The resulting residue was purified by silica gel chromatography (linear gradient 60-100% DCM in hexanes) to yield 5-bromo-6-chloro-N-[2-(2,4-dichlorophenoxy)phenyl]pyridine-3-sulfonamide, giving proton NMR and mass spectral data consistent with theory.

후처리

  1. washThe organic layer was washed successively with 100 mL of 0.5 M HCl, twice with 100 mL of water, 100 mL of half-saturated brine and finally 100 mL of brine
  2. dry with materialDrying of the organic layer over sodium sulfate
  3. filtrationwas followed by filtration and solvent removal under reduced pressure
  4. customThe resulting residue was purified by silica gel chromatography (linear gradient 60-100% DCM in hexanes)

출처 및 근거

ORD 기록
ord-6cdd4dbc66f34f7e8dffe72e4108591c
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07393873B2

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