(3,5-Difluorophenyl)hydrazine → HCID 18951060, 화합물

HRID 2248267노트

반응식

HRID 2248267 반응식
[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

참가 물질

6

반응물 2

HCID 2774213(3,5-Difluorophenyl)hydrazineHCID 14130443HCID 14130443, 화합물

생성물 1

HCID 18951060HCID 18951060, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b16b6b12cb1a418e82a3669b5656097f
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05039670

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