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Dichloromethane → HCID 676779, 화합물

HRID 336393
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인쇄 미리보기

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HRID 336393 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](Br)[N:3]=1.[CH2:9]([O:11][C:12]([N:14]=[C:15]=[S:16])=[O:13])[CH3:10].Cl[CH2:18]Cl>>[CH2:9]([O:11][C:12](=[O:13])[NH:14][C:15](=[S:16])[NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:18])[N:3]=1)[CH3:10]
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참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 85320Ethyl isothiocyanatoformateHCID 3008092-Amino-6-bromopyridine

생성물 1

HCID 676779HCID 676779, 화합물

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온도
24 °C

실험 절차

To an ice-cooled solution of 2-amino-6-bromopyridine (25.0 g, 0.144 mmol, 1 equiv) in dichloromethane (400 mL) was added ethoxycarbonyl isothiocyanate (19.9 g, 0.152 mmol, 1.05 equiv) dropwise. The reaction mixture was warmed to 24° C. After 21 h, the reaction mixture was concentrated in vacuo (˜20 mm Hg). The residue was diluted with ethyl acetate (600 mL), and the resulting organic solution was washed sequentially with water (2×200 mL) and saturated aqueous sodium chloride solution (200 mL). The organic was dried over magnesium sulfate, filtered, and concentrated to afford product as a yellow solid (43.7 g).

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo (˜20 mm Hg)
  2. additionThe residue was diluted with ethyl acetate (600 mL)
  3. washthe resulting organic solution was washed sequentially with water (2×200 mL) and saturated aqueous sodium chloride solution (200 mL)
  4. dry with materialThe organic was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3ff5b1e31401482e9dd1a643e7507641
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889673B2

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