Hydrochloric Acid → HCID 54423814、化合物

HRID 248748

反応式

HRID 248748 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 54423814HCID 54423814、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d18b19c5760f4c7a9fe769c7ee4fafca
出典データセット
uspto-grants-1993_05
特許番号
US05210290

関連ノート

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