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

HRID 2229304ノート

反応式

HRID 2229304 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 107267696-Chloro-N-ethyl-3-nitropyridin-2-amine収率 80%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b7a259db5f014ce68be845f972306556
出典データセット
uspto-grants-2002_07
特許番号
US06420359B1

反応ノート

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