Dichloromethane → HCID 59683173、化合物

HRID 548959

反応式

HRID 548959 の反応式
C(O)(=O)C.C(O)(=O)C.I(C1C=CC=CC=1)=O.[CH3:17][S:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1.Cl[C:29]1[CH:30]=[C:31]([S:35]([NH2:38])(=[O:37])=[O:36])[CH:32]=[N:33][CH:34]=1.[O-2].[Mg+2].[Cl:41]CCl>CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.[Rh+2].[Rh+2]>[CH3:17][S:18]([C:19]1[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=1)=[N:38][S:35]([C:31]1[CH:32]=[N:33][CH:34]=[CH:29][C:30]=1[Cl:41])(=[O:37])=[O:36]

参加物

7

反応物 5

HCID 6344DichloromethaneHCID 961094-Nitrophenyl methyl sulfideHCID 6850729Magnesium monoxideHCID 545947065-Chloropyridine-3-sulfonamideHCID 73357407Acetic acid;iodosylbenzene

生成物 1

HCID 59683173HCID 59683173、化合物収率 46%

試薬・触媒・溶媒 1

HCID 152122Dirhodium tetraacetate触媒

実験手順

879 mg (2.73 mmol) of iodosobenzene diacetate are added to a suspension of 300 mg (1.77 mmol) of 1-methylsulphanyl-4-nitrobenzene, 683 mg (3.55 mmol) of 5-chloro-3-pyridinesulphonamide, 285 mg (7.10 mmol) of magnesium oxide and 78 mg (0.18 mmol) of rhodium(II) acetate dimer in 12 ml of dichloromethane at room temperature. The mixture is stirred for 24 h and then concentrated. The resulting residue is purified by chromatography (dichloromethane/ethanol 95:5). 294 mg (0.82 mmol; yield: 46%) of the product are obtained.

後処理

  1. concentrationconcentrated
  2. customThe resulting residue is purified by chromatography (dichloromethane/ethanol 95:5)
  3. custom294 mg (0.82 mmol; yield: 46%) of the product are obtained

出典と根拠

ORDレコード
ord-5c9938856bf541adb341dac74ee22871
出典データセット
uspto-grants-2011_05
特許番号
US07943629B2

関連ノート

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