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Toluene → 2,4,6-Trimethoxyphenyl isocyanate

HRID 1198044
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HRID 1198044 반응식
[C:1](Cl)(Cl)=[O:2].C1(C)C=CC=CC=1.[CH3:12][O:13][C:14]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([O:23][CH3:24])[C:15]=1[NH2:16]>>[CH3:24][O:23][C:17]1[CH:18]=[C:19]([O:21][CH3:22])[CH:20]=[C:14]([O:13][CH3:12])[C:15]=1[N:16]=[C:1]=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1140TolueneHCID 6371PhosgeneHCID 842712,4,6-Trimethoxyaniline

생성물 1

HCID 100818122,4,6-Trimethoxyphenyl isocyanate

실험 절차

To a heated solution (70° C.) of phosgene in toluene (12.5% solution, 230 ML, 2.5 eq), 2,4,6-trimethoxyaniline (25.0 g, 0.113 mol) was added portionwise. The reaction mixture was heated to reflux for 4 hours and then stirred at room temperature for 16 hours. The reaction mixture then concentrated in vacuo. The residue was rinsed two times with ether and concentrated in vacuo. Ether was again added to the residue and cooled in an ice bath for 2 hours. The solid was filtered, rinsed with ether, and oven-dried to yield the desired product.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 4 hours
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • concentrationThe reaction mixture then concentrated in vacuo
  • washThe residue was rinsed two times with ether
  • concentrationconcentrated in vacuo
  • additionEther was again added to the residue
  • temperaturecooled in an ice bath for 2 hours
  • filtrationThe solid was filtered
  • washrinsed with ether
  • customoven-dried
  • 출처 및 근거

    ORD 기록
    ord-6afa455981c24d40916782b62e6e1e3a
    출처 데이터셋
    uspto-grants-1994_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05278326

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