Water → 6-Chloro-N-ethyl-3-nitropyridin-2-amine

HRID 2229304노트

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HRID 2229304 반응식
[CH2:1]([NH2:3])[CH3:2].Cl[C:5]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[C:7]([Cl:14])[N:6]=1.O.CCOC(C)=O>C1(C)C=CC=CC=1>[Cl:14][C:7]1[N:6]=[C:5]([NH:3][CH2:1][CH3:2])[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6341EthylamineHCID 8857Ethyl AcetateHCID 852392,6-Dichloro-3-nitropyridine

생성물 1

HCID 107267696-Chloro-N-ethyl-3-nitropyridin-2-amine수율 80%

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
0 °C

실험 절차

An ice-cold solution of EtNH2 (49.8 g, 1.10 mol) in toluene (200 mL) was added over 15 min to an ice-cold solution of 2,6-dichloro-3-nitropyridine (100.0 g, 0.52 mol) in toluene (225 mL). The mixture was stirred at 0° C. for 45 min. Water (500 mL) and EtOAc (500 mL) were added and the phases were separated. The organic layer was successively washed with water (200 mL) and brine (200 mL), dried (MgSO4), filtered and concentrated under reduced pressure. The residual solid was recrystallised from MeOH to give the title compound (83.7 g, 80% yield) as yellow needles.

후처리

  1. customthe phases were separated
  2. washThe organic layer was successively washed with water (200 mL) and brine (200 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residual solid was recrystallised from MeOH

출처 및 근거

ORD 기록
ord-b7a259db5f014ce68be845f972306556
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06420359B1

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