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

HRID 2094
ノート
印刷プレビュー

反応式

HRID 2094 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 542023254-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone収率 81.5%

試薬・触媒・溶媒 1

HCID 8058
Hexane
溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-71fa5a93fb9c483491defb7a5b1de773
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728699

反応ノート

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