4-Methylbenzenethiol → HCID 88076664, 화합물

HRID 397603

반응식

HRID 397603 반응식
[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]

참가 물질

5

반응물 2

HCID 78114-MethylbenzenethiolHCID 682512,4-Dinitrobenzenesulfenyl chloride

생성물 1

HCID 88076664HCID 88076664, 화합물수율 31.8%

시약·촉매·용매 2

HCID 23954Silver촉매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6754866044f34132be81ff2175324272
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610708B1

연결된 노트

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