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Ethanol → 3-Methoxy-5-nitropyridin-2-amine

HRID 2102972
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HRID 2102972 반응식
Cl[C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([N+:10]([O-:12])=[O:11])=[CH:4][N:3]=1.[OH-].[NH4+:14].C(O)C>C(OCC)(=O)C>[NH2:14][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([N+:10]([O-:12])=[O:11])=[CH:4][N:3]=1
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참가 물질

5

반응물 3

HCID 702EthanolHCID 14923Ammonium HydroxideHCID 234561522-Chloro-3-methoxy-5-nitropyridine

생성물 1

HCID 534257863-Methoxy-5-nitropyridin-2-amine수율 69.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

Into a 250 mL sealed tube were combined 2-chloro-3-methoxy-5-nitropyridine (0.50 g, 0.00265 mol), concentrated ammonium hydroxide (5 mL, 0.1 mol) and ethanol (20 mL). The mixture was heated to 80° C. and stirred overnight. After allowing to cool to room temperature, the mixture was reduced in vacuo and the residue was taken up in ethyl acetate (50 mL), then washed with equal amounts of brine and water (1×50 mL each). The organic layer was dried (Na2SO4), filtered and concentrated under vacuum to leave a solid (0.312 g, 69%) which was used directly in the next step without further purification. LC-MS 1.94 min. M/Z=171.0 (M+1).

후처리

  1. customInto a 250 mL sealed tube
  2. temperatureto cool to room temperature
  3. washwashed with equal amounts of brine and water (1×50 mL each)
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-3b485eb12c0744e08ea1c090e28131d3
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576099B2

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