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Ethyl isothiocyanatoformate → 1-(6-Bromo-4-methyl-pyridin-2-yl)-3-carboethoxy-thiourea

HRID 1054414
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HRID 1054414 반응식
[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([CH3:9])[CH:3]=1.[CH2:10]([O:12][C:13]([N:15]=[C:16]=[S:17])=[O:14])[CH3:11]>ClCCl>[Br:1][C:2]1[N:7]=[C:6]([NH:8][C:16]([NH:15][C:13]([O:12][CH2:10][CH3:11])=[O:14])=[S:17])[CH:5]=[C:4]([CH3:9])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 85320Ethyl isothiocyanatoformateHCID 221765076-Bromo-4-methylpyridin-2-amine

생성물 1

HCID 595897291-(6-Bromo-4-methyl-pyridin-2-yl)-3-carboethoxy-thiourea

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 6-bromo-4-methyl-pyridin-2-ylamine (0.5 g, 2.67 mmol) in dichloromethane (20 ml) cooled to 5° C. was added ethoxycarbonyl isothiocyanate (0.32 ml, 2.67 mmol) dropwise over 15 min. The reaction mixture was then allowed to warm to room temperature at which it was stirred for 16 h. Evaporation in vacuo gave a solid that was collected by filtration and thoroughly washed with cyclohexane to give the desired product. Yield 0.59 g, 69%. LCMS MI: 317.92+319.94, RT: 5.05 min, Method: 2

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후처리

  1. customEvaporation in vacuo
  2. customgave a solid
  3. filtrationthat was collected by filtration
  4. washthoroughly washed with cyclohexane

출처 및 근거

ORD 기록
ord-768be8c3b38d4450ba8dd3ffeb5f28a7
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394301B2

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