(3,5-Difluorophenyl)hydrazine → HCID 18951060、化合物

HRID 2371858ノート

反応式

HRID 2371858 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:9]N)[CH:5]=[C:6]([F:8])[CH:7]=1.[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([NH:21][CH:22]2[CH2:27][CH2:26][C:25](=O)[CH2:24][CH2:23]2)(=[O:20])=[O:19])=[CH:14][CH:13]=1>C(O)C.S(=O)(=O)(O)O.O>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([NH:21][CH:22]2[CH2:23][C:24]3[C:3]4[C:4](=[CH:5][C:6]([F:8])=[CH:7][C:2]=4[F:1])[NH:9][C:25]=3[CH2:26][CH2:27]2)(=[O:20])=[O:19])=[CH:14][CH:13]=1

参加物

6

反応物 2

HCID 2774213(3,5-Difluorophenyl)hydrazineHCID 14130443HCID 14130443、化合物

生成物 1

HCID 18951060HCID 18951060、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

14.0 g (97 mmol) of the compound of Example I and 27.95 g (97 mmol) of 4-chloro-N-(4-oxo-cyclohexyl)-benzenesulphonamide are refluxed for 5 hours in 190 ml of ethanol and 36 ml of concentrated sulphuric acid, then the mixture is cooled and diluted with 300 ml of water. The mixture is extracted 4 times using 250 ml of ethyl acetate each time, and the organic phase is dried using sodium sulphate, filtered with suction over kieselguhr and evaporated. The residue is stirred with methylene chloride and dried in a high vacuum.

後処理

  1. extractionThe mixture is extracted 4 times
  2. customthe organic phase is dried
  3. filtrationfiltered with suction over kieselguhr
  4. customevaporated
  5. customdried in a high vacuum

出典と根拠

ORDレコード
ord-a40faf6164f1489c9556944fb555b827
出典データセット
uspto-grants-1992_03
特許番号
US05096897

反応ノート

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