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1,4-Butanediol → 5-bromo-4-chloro-2-(4-hydroxy-butoxy)-N-methyl-N-pyridin-2-yl-benzenesulfonamide

HRID 2382713
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HRID 2382713 반응식
[CH2:1]([OH:6])[CH2:2][CH2:3][CH2:4][OH:5].[H-].[Na+].[Br:9][C:10]1[C:11]([Cl:28])=[CH:12][C:13](F)=[C:14]([S:16]([N:19]([CH3:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)(=[O:18])=[O:17])[CH:15]=1>CN(C=O)C>[Br:9][C:10]1[C:11]([Cl:28])=[CH:12][C:13]([O:5][CH2:4][CH2:3][CH2:2][CH2:1][OH:6])=[C:14]([S:16]([N:19]([CH3:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)(=[O:17])=[O:18])[CH:15]=1
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참가 물질

5

반응물 3

HCID 80641,4-ButanediolHCID 24758Sodium hydrideHCID 684721885-bromo-4-chloro-2-fluoro-N-methyl-N-pyridin-2-yl-benzenesulfonamide

생성물 1

HCID 684685195-bromo-4-chloro-2-(4-hydroxy-butoxy)-N-methyl-N-pyridin-2-yl-benzenesulfonamide수율 96.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
50 °C

실험 절차

To a solution of 1,4-butanediol (0.315 mL, 3.6 mmol) in DMF (2.5 mL) at ambient temperature was added sodium hydride (60%, 34 mg, 0.85 mmol) and the mixture was stirred for 15 minutes. A solution of 5-bromo-4-chloro-2-fluoro-N-methyl-N-pyridin-2-yl-benzenesulfonamide (0.268 g, 0.71 mmol) in DMF (2.5 mL) was added and the mixture heated at 50° C. for 2 h. The solvent was removed in vacuo and water and DCM were added. The mixture was extracted with DCM. The organic layer was washed with brine and was dried over anhydrous MgSO4. Concentration of the filtrate provided a residue that was purified by silica gel chromatography [eluent: 50% ethyl acetate in hexane] to afford 5-bromo-4-chloro-2-(4-hydroxy-butoxy)-N-methyl-N-pyridin-2-yl-benzenesulfonamide as a solid (0.309 g). MS: 451.0 (M+H)+; tR=2.59 min (method 1).

후처리

  1. customThe solvent was removed in vacuo and water and DCM
  2. additionwere added
  3. extractionThe mixture was extracted with DCM
  4. washThe organic layer was washed with brine
  5. dry with materialwas dried over anhydrous MgSO4
  6. customConcentration of the filtrate provided a residue that
  7. customwas purified by silica gel chromatography [eluent: 50% ethyl acetate in hexane]

출처 및 근거

ORD 기록
ord-663c6000ddc741a292521aeb4fe61ebc
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08263588B2

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