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2,4-Dinitrotoluene → Dimethyl 4-methyl-1,3-phenylenedicarbamate

HRID 1618322
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인쇄 미리보기

반응식

HRID 1618322 반응식
[C:1](=[O:6])([O:4][CH3:5])OC.[N+:7]([C:10]1[CH:15]=[C:14]([N+:16]([O-])=O)[CH:13]=[CH:12][C:11]=1[CH3:19])([O-])=O>>[CH3:5][O:4][C:1]([NH:7][C:10]1[CH:15]=[C:14]([NH:16][C:1]([O:4][CH3:5])=[O:6])[CH:13]=[CH:12][C:11]=1[CH3:19])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 84612,4-DinitrotolueneHCID 12021Dimethyl Carbonate

생성물 1

HCID 235307Dimethyl 4-methyl-1,3-phenylenedicarbamate수율 63%

실험 절차

In a 5 ml reinforced glass flask capable of pressure sealing dimethyl carbonate (2 ml), 2,4-dinitrotoluene (150 mg), the Au/CeO2 catalyst (100 mg, 1 wt % gold relative to cerium) are placed, and the reactor is closed. After purging with N2 for 5 minutes, the reactor is loaded with hydrogen gas at a pressure of 15 bars. The reactor is immersed in a silicone bath preheated at 150° C. and the mixture is magnetically stirred for 23 hrs. After this time, the reactor is brought to atmospheric pressure and opened. The catalyst is filtered and the liquid phase is analyzed by gas chromatography. The disappearance of 2,4-dinitrotoluene and the formation of 2,4-bis(methoxycarbonylamino) toluene in a 63% yield is observed. Smaller amounts (20%) of ortho and para mixtures of the mono carbamoylate 2,4-diaminotoluene derivative are detected.

후처리

  • customthe reactor is closed
  • customAfter purging with N2 for 5 minutes
  • customThe reactor is immersed in a silicone bath
  • custompreheated at 150° C.
  • filtrationThe catalyst is filtered
  • 출처 및 근거

    ORD 기록
    ord-813178f784b143ccbd11290cdaaef5ba
    출처 데이터셋
    uspto-grants-2014_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08765993B2

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