2,3-Dimethylaniline → 2,3-Dimethyl-(1-thiaethyl)-benzene

HRID 49684

반응식

HRID 49684 반응식
N(OC(C)(C)C)=O.[CH3:8][C:9]1[C:15]([CH3:16])=[CH:14][CH:13]=[CH:12][C:10]=1N.[CH3:17][S:18]SC>[Cu]>[CH3:8][C:9]1[C:15]([CH3:16])=[CH:14][CH:13]=[CH:12][C:10]=1[S:18][CH3:17]

참가 물질

5

반응물 3

HCID 68932,3-DimethylanilineHCID 10906Tert-Butyl nitriteHCID 12232Dimethyl Disulfide2회

생성물 1

HCID 214853032,3-Dimethyl-(1-thiaethyl)-benzene

시약·촉매·용매 1

HCID 23978Copper촉매

반응 조건

온도
77.5 °C

실험 절차

355 g (3.44 mol) of tert-butyl nitrite and 250 g of copper powder (3.9 mol) are initially charged in 1250 ml of dimethyl disulfide, and a solution of 250 g (2.07 mol) of 2,3-dimethylaniline in 1000 ml of dimethyl disulfide is added dropwise at 50-52° C. The mixture is subsequently stirred at 75-80° C. for 1.5 hours. For work-up, the mixture is cooled, filtered off with suction through kieselguhr, and the filtrate is washed with saturated aqueous NaHCO3 solution. For the purification of the product, the organic phase is separated by distillation. Initially, excess dimethyl disulfide is removed at atmospheric pressure. 1446 g of dimethyl disulfide (purity>97% according to GC) are recovered. The residue is then subjected to fractional distillation under reduced pressure (0.1 mbar).

후처리

  1. temperatureFor work-up, the mixture is cooled
  2. filtrationfiltered off with suction through kieselguhr
  3. washthe filtrate is washed with saturated aqueous NaHCO3 solution
  4. customFor the purification of the product
  5. customthe organic phase is separated by distillation
  6. customInitially, excess dimethyl disulfide is removed at atmospheric pressure
  7. custom1446 g of dimethyl disulfide (purity>97% according to GC) are recovered
  8. distillationThe residue is then subjected to fractional distillation under reduced pressure (0.1 mbar)

출처 및 근거

ORD 기록
ord-f14d107e81204a399d3161868f91fb0d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706886B2

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