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Ammonium Hydroxide → 6-chloropyridine-3-sulfonamide

HRID 237352
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HRID 237352 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[OH-].[NH4+:13]>CCOC(C)=O>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:13])(=[O:10])=[O:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 27927922-Chloro-5-pyridinesulfonyl chloride

생성물 1

HCID 12015126-chloropyridine-3-sulfonamide수율 69%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

6-chloropyridine-3-sulfonyl chloride (4.1 g, 19.3 mmol) was stirred in ammonium hydroxide (30 mL) at room temperature for 2 hr. The reaction mixture was diluted with EtOAc (150 mL) and any insoluble material filtered. The filtrate was transferred to a separatory funnel and the phases were separated. The aqueous phase was further extracted with EtOAc (1×15 mL). The combined EtOAc extractions were washed with H2O (1×50 mL), saturated NaCl (1×50 mL), dried (Na2SO4), and concentrated in vacuo to give 6-chloropyridine-3-sulfonamide (2.58 g, 69%). MS (EI) for C5H3Cl2NO2S: 190.9 (MH−).

후처리

  1. filtrationany insoluble material filtered
  2. customThe filtrate was transferred to a separatory funnel
  3. customthe phases were separated
  4. extractionThe aqueous phase was further extracted with EtOAc (1×15 mL)
  5. extractionThe combined EtOAc extractions
  6. washwere washed with H2O (1×50 mL), saturated NaCl (1×50 mL)
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d0a5d626b1514eddb4af7c93484118c7
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642584B2

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