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Hydrochloric Acid → N-(4-fluoro-3-nitrophenyl)benzenesulfonamide

HRID 840094
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인쇄 미리보기

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HRID 840094 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[C:12]1([S:18](Cl)(=[O:20])=[O:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.Cl>N1C=CC=CC=1>[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][S:18]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:20])=[O:19])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7369Benzenesulfonyl chlorideHCID 677684-Fluoro-3-nitroaniline

생성물 1

HCID 4599069N-(4-fluoro-3-nitrophenyl)benzenesulfonamide

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
10 °C

실험 절차

4-fluoro-3-nitro-aniline (7.8 g, 50 mmol) is taken up in 50 mL pyridine and cooled to 10° C. The benzenesulphonic acid chloride (7.0 mL, about 55 mmol) is added dropwise with stirring within about 20 min at 10-20° C. The mixture is stirred for about 0.5 h at ambient temperature and poured onto ice water. After acidifying with conc. hydrochloric acid the mixture is extracted with 150 mL ethyl acetate, washed with water, dried and concentrated by evaporation. The residue is dissolved in diethylether, diluted with petroleum ether and cooled. The crystals formed are filtered off, washed with diethylether/petroleum ether and dried.

후처리

  1. stirringThe mixture is stirred for about 0.5 h at ambient temperature
  2. additionpoured onto ice water
  3. extractionis extracted with 150 mL ethyl acetate
  4. washwashed with water
  5. customdried
  6. concentrationconcentrated by evaporation
  7. dissolutionThe residue is dissolved in diethylether
  8. additiondiluted with petroleum ether
  9. temperaturecooled
  10. customThe crystals formed
  11. filtrationare filtered off
  12. washwashed with diethylether/petroleum ether
  13. customdried

출처 및 근거

ORD 기록
ord-650ab8ffa741407f9a92a82023744ad0
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06365584B1

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