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Ammonium → 2-Fluoro-5-(4-methoxy-benzoyl)-benzenesulfonamide

HRID 873623
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HRID 873623 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)=[CH:4][C:3]=1[S:18](Cl)(=[O:20])=[O:19].[NH4+:22]>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)=[CH:4][C:3]=1[S:18]([NH2:22])(=[O:20])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 223AmmoniumHCID 581074472-Fluoro-5-(4-methoxy-benzoyl)-benzenesulfonyl chloride

생성물 1

HCID 442352782-Fluoro-5-(4-methoxy-benzoyl)-benzenesulfonamide수율 32%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-fluoro-5-(4-methoxy-benzoyl)-benzenesulfonyl chloride (0.45 g, 1.0 mmol) in methylene chloride is added aqueous ammonium solution (1 mL). The reaction mixture is stirred for 10 min at room temperature. The solvent is removed and the residue is redissolved in ethyl acetate and extracted with water. The organic layers are washed with a saturated sodium chloride solution, dried with magnesium sulfate, and concentrated in vacuo. The residue is recrystallized with methylene chloride-hexane to give 100 mg (32% yield) of the title compound as pale yellow solid. 1H NMR (CDCl3): δ 8.40 (m, 1H), 8.05 (m, 1H), 7.80 (d, J=8 Hz, 2H), 7.32 (t, 1H), 7.00 (d, J=8 Hz, 2H), 5.15 (s, 1H), 3.90 (s, 3H). Analytics calculated for C14H12FNO4S: C, 54.36; H, 3.91; N, 4.53. Found: C, 53.89; H, 3.50; N, 4.50.

후처리

  1. customThe solvent is removed
  2. dissolutionthe residue is redissolved in ethyl acetate
  3. extractionextracted with water
  4. washThe organic layers are washed with a saturated sodium chloride solution
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue is recrystallized with methylene chloride-hexane

출처 및 근거

ORD 기록
ord-5ece9546d2dc454faff3b27f80ad36b4
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975439B2

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