4-Methylbenzenethiol → HCID 88076664、化合物

HRID 397603

反応式

HRID 397603 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[N+:9]([C:12]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=1SCl)([O-:11])=[O:10]>C(#N)C.[Ag]>[N+:9]([C:12]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=1[C:7]1[CH:6]=[C:5]([S:8][S:8][C:5]2[CH:4]=[CH:3][C:2]([CH3:1])=[C:7]([C:13]3[CH:14]=[CH:15][C:16]([N+:18]([O-:20])=[O:19])=[CH:17][C:12]=3[N+:9]([O-:11])=[O:10])[CH:6]=2)[CH:4]=[CH:3][C:2]=1[CH3:1])([O-:11])=[O:10]

参加物

5

反応物 2

HCID 78114-MethylbenzenethiolHCID 682512,4-Dinitrobenzenesulfenyl chloride

生成物 1

HCID 88076664HCID 88076664、化合物収率 31.8%

試薬・触媒・溶媒 2

HCID 23954Silver触媒HCID 6342Acetonitrile溶媒

実験手順

In a nitrogen atmosphere, 3.70 g (16.0 mmol) of the silver salt of p-thiocresol and 3.75 g (16.0 mmol) of 2,4-dinitrophenylsulfenyl chloride were stirred for 3 hours in 150 ml of acetonitrile serving as a solvent, while cooling with ice water. The reaction mixture was filtered and the residue obtained after the concentration of the filtrate under reduced pressure was subjected to chromatography on a silica gel column (eluting solvent: hexane/ethyl acetate=5/1), whereby 1.64 g (5.08 mmol, yield: 31.8%) of 2,4-dinitrophenyl p-tolyldisulfide were obtained as yellow crystals.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe residue obtained after the concentration of the filtrate under reduced pressure
  3. washwas subjected to chromatography on a silica gel column (eluting solvent: hexane/ethyl acetate=5/1)

出典と根拠

ORDレコード
ord-6754866044f34132be81ff2175324272
出典データセット
uspto-grants-2003_08
特許番号
US06610708B1

関連ノート

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