Water → 4-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone

HRID 2094

반응식

HRID 2094 반응식
[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([C:6](=[N:18][NH2:19])[C:7]2[CH:12]=[CH:11][C:10]([CH2:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.ClS([N:26]=[C:27]=[O:28])(=O)=O.C(OCC)(=O)C.O>CCCCCC>[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([C:6](=[N:18][NH:19][C:27]([NH2:26])=[O:28])[C:7]2[CH:8]=[CH:9][C:10]([CH2:13][S:14]([CH3:17])(=[O:15])=[O:16])=[CH:11][CH:12]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 70918Chlorosulfonyl isocyanateHCID 867522794-Chloro-4'-methylsulfonylmethylbenzophenone-hydrazone

생성물 1

HCID 542023254-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone수율 81.5%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

4-chloro-4'-methylsulfonylmethylbenzophenone-hydrazone (1.3 g) and chlorosulfonyl isocyanate (0.63 g) were added to ethyl acetate (100 ml), and the mixture was stirred for one hour at room temperature. Then, water (100 ml) was added, and the mixture was further stirred for 16 hours at room temperature. The reaction mixture was subjected to liquid separation, and the ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with a solvent mixture of ethyl acetate:n-hexane=4:1, to obtain the desired product (1.2 g, melting point: 189° to 191° C., yield: 80%).

후처리

  1. stirringthe mixture was further stirred for 16 hours at room temperature
  2. customThe reaction mixture was subjected to liquid separation
  3. washthe ethyl acetate layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationEthyl acetate was distilled off under reduced pressure
  6. washThe residual solid was washed with a solvent mixture of ethyl acetate

출처 및 근거

ORD 기록
ord-71fa5a93fb9c483491defb7a5b1de773
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728699

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