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2-Amino-5-chloropyridine → ethyl N-{[(5-chloro-2-pyridinyl)amino]carbothioyl}carbamate

HRID 1051867
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HRID 1051867 반응식
[CH2:1]([O:3][C:4]([N:6]=[C:7]=[S:8])=[O:5])[CH3:2].[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][N:11]=1>O1CCOCC1>[Cl:16][C:13]1[CH:14]=[CH:15][C:10]([NH:9][C:7]([NH:6][C:4](=[O:5])[O:3][CH2:1][CH3:2])=[S:8])=[N:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 661742-Amino-5-chloropyridineHCID 85320Ethyl isothiocyanatoformate

생성물 1

HCID 2768988ethyl N-{[(5-chloro-2-pyridinyl)amino]carbothioyl}carbamate수율 72.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Ethoxycarbonylisothiocyanate (3.37 g) was added to a stirred solution of 2-amino-5-chloropyridine (3.0 g) in dioxane (100 mL). The mixture was stirred at r.t. for 14 h. The solvent was removed in vacuum. The solid was dissolved in dichloromethane and methanol (100:1), filtered and the solvent was removed in vacuum to give a solid that was recrystallized from ethyl acetate to give 4.4 g of the title compound.

후처리

  1. customThe solvent was removed in vacuum
  2. dissolutionThe solid was dissolved in dichloromethane
  3. filtrationmethanol (100:1), filtered
  4. customthe solvent was removed in vacuum
  5. customto give a solid
  6. customthat was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-480fe829e8f345e6b252b489f35d79cf
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388177B2

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