Ethylenediamine → HCID 22142401、化合物

HRID 31750ノート

反応式

HRID 31750 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[CH2:12]([NH2:15])[CH2:13][NH2:14]>C(#N)C>[NH2:14][CH2:13][CH2:12][NH:15][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 3301EthylenediamineHCID 3453642-Chloro-4-methyl-5-nitropyridine

生成物 1

HCID 22142401HCID 22142401、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

2-Chloro-4-methyl-5-nitropyridine (2.0 g, 11.5 mmol) in acetonitrile (10 ml) was added dropwise to ethylenediamine (2.5 ml) in acetonitrile (10 ml). The mixture was stirred overnight at room temperature. The solvent was removed by rotary evaporation and the residue was partitioned between dichloromethane and 2.5 M aqueous sodium hydroxide. The aqueous layer was further extracted 4 times with dichloromethane. The combined organic layers were washed with a saturated sodium chloride solution, dried and concentrated in vacuo to give (2-aminoethyl)(4-methyl-5-nitro(2-pyridyl))amine as an orange solid (1.74 g).

後処理

  1. customThe solvent was removed by rotary evaporation
  2. customthe residue was partitioned between dichloromethane and 2.5 M aqueous sodium hydroxide
  3. extractionThe aqueous layer was further extracted 4 times with dichloromethane
  4. washThe combined organic layers were washed with a saturated sodium chloride solution
  5. customdried
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-fda66a26239646cbb517a662171c1af7
出典データセット
uspto-grants-2008_09
特許番号
US07425557B2

反応ノート

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