4-Nitrophenyl methyl sulfide → HCID 59683154、化合物

HRID 548958

反応式

HRID 548958 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.[CH3:28][C:29]1[CH:30]=[CH:31][C:32]([S:35]([NH2:38])(=[O:37])=[O:36])=[N:33][CH:34]=1.[O-2].[Mg+2]>ClCCl.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:32]1[CH:31]=[CH:30][C:29]([CH3:28])=[CH:34][N:33]=1)(=[O:37])=[O:36]

参加物

7

反応物 4

HCID 961094-Nitrophenyl methyl sulfideHCID 36141995-Methyl-2-pyridinesulfonamideHCID 6850729Magnesium monoxideHCID 73357407Acetic acid;iodosylbenzene

生成物 1

HCID 59683154HCID 59683154、化合物収率 54%

試薬・触媒・溶媒 2

HCID 152122Dirhodium tetraacetate触媒HCID 6344Dichloromethane溶媒

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, 610 mg (3.55 mmol) of 5-methyl-2-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). 326 mg (0.96 mmol; yield: 54%) of the product are obtained.

後処理

  1. concentrationconcentrated
  2. customThe resulting residue is purified by chromatography (dichloromethane/ethanol 95:5)
  3. custom326 mg (0.96 mmol; yield: 54%) of the product are obtained

出典と根拠

ORDレコード
ord-12623970122e4eeeab7da493dd147b95
出典データセット
uspto-grants-2011_05
特許番号
US07943629B2

関連ノート

読み込み中…