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Ethyl isothiocyanatoformate → HCID 57643101, 화합물

HRID 1802146
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HRID 1802146 반응식
[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=1.[CH2:9]([O:11][C:12]([N:14]=[C:15]=[S:16])=[O:13])[CH3:10]>O1CCOCC1>[CH2:9]([O:11][C:12]([NH:14][C:15]([NH:8][C:4]1[CH:3]=[C:2]([Br:1])[CH:7]=[CH:6][N:5]=1)=[S:16])=[O:13])[CH3:10]
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참가 물질

4

반응물 2

HCID 85320Ethyl isothiocyanatoformateHCID 6932822-Amino-4-bromopyridine

생성물 1

HCID 57643101HCID 57643101, 화합물수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
25 °C

실험 절차

To a solution of 4-bromopyridin-2-amine (10.4 g, 60.1 mmol) in dioxane (242 ml) is added ethoxycarbonyl isothiocyanate (7.88 g, 6.8 ml, 60.1 mmol) at 25° C. The resulting mixture is stirred for 4 hours at 25° C. The solvent is evaporated, the solid yellow residue diluted with ethyl acetate and washed with water and brine. The organic layer is separated, dried over magnesium sulfate and the solvent is removed in vacuo affording 1-ethoxycarbonyl-3-(4-bromo-pyridin-2-yl)-thiourea (17.37 g, 95%) as a yellow solid. mp.: 107-110° C. MS: m/z=304.0, 305.9 (M+H+).

후처리

  1. customThe solvent is evaporated
  2. additionthe solid yellow residue diluted with ethyl acetate
  3. washwashed with water and brine
  4. customThe organic layer is separated
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-c39dcad35cdd4f38a584371c947837d0
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08349824B2

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