Hydrochloric Acid → N-(2,5-difluorophenyl)benzenesulfonamide

HRID 4234

반응식

HRID 4234 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:3]=1[NH2:4].N1C=CC=CC=1.[C:16]1([S:22](Cl)(=[O:24])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.Cl>O>[F:1][C:2]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:3]=1[NH:4][S:22]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:24])=[O:23]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7369Benzenesulfonyl chlorideHCID 677752,5-Difluoroaniline

생성물 1

HCID 8500589N-(2,5-difluorophenyl)benzenesulfonamide

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

0.194 mole (25 g) of 2,5-difluoroaniline is added to 125 ml of pyridine. 0.2 mole (25.5 ml) of benzenesulphonyl chloride is added, while the temperature is between 35° C. and 45° C. The temperature is maintained at 40° C. for 1 hour after the addition is completed, and then the reaction mixture is poured onto 1 kg of ice and water to which 100 ml of concentrated hydrochloric acid have been added. The expected product precipitates. After filtration and washing, it is treated with a normal sodium hydroxide solution in order to remove insoluble material. The soda-containing filtrate is neutralized with concentrated hydrochloric acid. The expected product, which has precipitated, is filtered off, washed to neutrality and recrystallized from acetic acid. It melts at 115° C.

후처리

  1. customis between 35° C. and 45° C
  2. additionafter the addition
  3. additionhave been added
  4. customThe expected product precipitates
  5. filtrationAfter filtration
  6. washwashing
  7. additionit is treated with a normal sodium hydroxide solution in order
  8. customto remove insoluble material
  9. customThe expected product, which has precipitated
  10. filtrationis filtered off
  11. washwashed to neutrality
  12. customrecrystallized from acetic acid

출처 및 근거

ORD 기록
ord-3dbdfcae709944628a41bf0158fca242
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725283

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