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Methoxycarbonyl isothiocyanate → 1,2-Bis(3-methoxycarbonyl-2-thioureido)-4-methylthiomethoxybenzene

HRID 616107
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반응식

HRID 616107 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][S:10][CH3:11])=[CH:4][C:3]=1[NH2:12].[CH3:13][O:14][C:15]([N:17]=[C:18]=[S:19])=[O:16]>CC(C)=O>[CH3:13][O:14][C:15]([NH:17][C:18](=[S:19])[NH:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][S:10][CH3:11])=[CH:4][C:3]=1[NH:12][C:18]([NH:17][C:15]([O:14][CH3:13])=[O:16])=[S:19])=[O:16]
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참가 물질

4

반응물 2

HCID 552246Methoxycarbonyl isothiocyanateHCID 203628424-[(Methylsulfanyl)methoxy]benzene-1,2-diamine

생성물 1

HCID 203710021,2-Bis(3-methoxycarbonyl-2-thioureido)-4-methylthiomethoxybenzene

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

The 1,2-diamino-4-methylthiomethoxybenzene prepared above is dissolved in 60 ml. acetone and treated overnight with 6 g. methoxycarbonyl isothiocyanate at room temperature. The mixture is concentrated and the residue stirred with 500 ml. water and the brown solid filtered off. The residue is extracted with 250 ml. dichloromethane, filtered, treated with charcoal, and recrystallized from dichloromethanebenzene to afford 1,2-bis(3-methoxycarbonyl-2-thioureido)-4-methylthiomethoxybenzene.

후처리

  1. dissolutionis dissolved in 60 ml
  2. customat room temperature
  3. concentrationThe mixture is concentrated
  4. filtrationwater and the brown solid filtered off
  5. extractionThe residue is extracted with 250 ml
  6. filtrationdichloromethane, filtered
  7. additiontreated with charcoal
  8. customrecrystallized from dichloromethanebenzene

출처 및 근거

ORD 기록
ord-0d11de04ce33462ca3515167d02c7b58
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04072696

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