Hydrochloric Acid → HCID 54423814, 화합물

HRID 248748

반응식

HRID 248748 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1.[CH3:13][O:14][C:15](=[O:22])[CH2:16][CH2:17][S:18](Cl)(=[O:20])=[O:19].ClC(Cl)C.Cl>N1C=CC=CC=1>[CH3:13][O:14][C:15](=[O:22])[CH2:16][CH2:17][S:18](=[O:20])(=[O:19])[NH:6][C:5]1[CH:7]=[CH:8][C:2]([F:1])=[CH:3][C:4]=1[C:9]([F:10])([F:11])[F:12]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 63651,1-DichloroethaneHCID 678534-Fluoro-2-(trifluoromethyl)anilineHCID 4962888Methyl 3-(chlorosulfonyl)propanoate

생성물 1

HCID 54423814HCID 54423814, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

8.96 g (50 mmol) of 4-fluoro-2-trifluoromethylaniline is dissolved in 100 ml of pyridine and under cold conditions combined under stirring with 9.52 g (50 mmol) of 3-chlorosulfonylpropionic acid methyl ester (98.5%). The mixture is agitated for 20 minutes, heated for 4 hours to 40° C., and the pyridine is exhausted under vacuum. The residue is distributed between dichloroethane and 4N hydrochloric acid. The organic solution is washed with water, dried over sodium sulfate, and concentrated to dryness under vacuum. The residue is purified by column chromatrography on silica gel. The title compound is eluted with ethyl acetate.

후처리

  1. temperatureheated for 4 hours to 40° C.
  2. washThe organic solution is washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated to dryness under vacuum
  5. customThe residue is purified by column chromatrography on silica gel
  6. washThe title compound is eluted with ethyl acetate

출처 및 근거

ORD 기록
ord-d18b19c5760f4c7a9fe769c7ee4fafca
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210290

연결된 노트

불러오는 중…