Ethanesulfonyl chloride → N-(4-fluoro-3-nitrophenyl)ethanesulfonamide

HRID 36793

반응식

HRID 36793 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].[CH2:12]([S:14](Cl)(=[O:16])=[O:15])[CH3:13]>N1C=CC=CC=1>[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][S:14]([CH2:12][CH3:13])(=[O:16])=[O:15])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10]

참가 물질

4

반응물 2

HCID 11667Ethanesulfonyl chlorideHCID 677684-Fluoro-3-nitroaniline

생성물 1

HCID 3286362N-(4-fluoro-3-nitrophenyl)ethanesulfonamide수율 93%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

20.2 g (0.129 mol) of 4-fluoro-3-nitroaniline was dissolved in 120 ml of pyridine, and 17.8 g (0.136 mol) of ethanesulfonyl chloride was added dropwise to the solution at a temperature of not higher than 5° C. Thereafter the temperature was raised to room temperature and the reaction was continued for one night. After the pyridine was distilled off, the thus-obtained product was dissolved in ethyl acetate and washed with diluted hydrochloric acid twice, then with water, and with saturated saline solution. The solution was dried over anhydrous sodium sulfate, and the ethyl acetate was distilled off to obtain the crude product (crystals). The crude product was washed with diisopropyl ether, thereby obtaining 29.7 g of the objective product (yield: 93%) in the form of brown crystals. Melting point: 133° to 136° C.

후처리

  1. waitthe reaction was continued for one night
  2. distillationAfter the pyridine was distilled off
  3. dissolutionthe thus-obtained product was dissolved in ethyl acetate
  4. washwashed with diluted hydrochloric acid twice
  5. dry with materialThe solution was dried over anhydrous sodium sulfate
  6. distillationthe ethyl acetate was distilled off
  7. customto obtain the crude product (crystals)
  8. washThe crude product was washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-0de8c25ef53b4f38b1dc4201c18a173f
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416236

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