Ethylenediamine → (2-Aminoethyl)(4-methyl-5-nitro(2-pyridyl))amine

HRID 2228597ノート

反応式

HRID 2228597 の反応式
Cl[C:2]1N=[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:16](#N)C>>[NH2:14][CH2:13][CH2:12][NH:15][C:2]1[CH:8]=[C:6]([CH3:16])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1

参加物

4

反応物 3

HCID 3301EthylenediamineHCID 6342Acetonitrile2 回HCID 184699642-Chloro-4-methyl-5-nitropyrimidine

生成物 1

HCID 22142401(2-Aminoethyl)(4-methyl-5-nitro(2-pyridyl))amine

実験手順

2-Chloro-4-methyl-5-nitropyrimidine (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-7936208f04e84b9db4d7fad817585762
出典データセット
uspto-grants-2002_07
特許番号
US06417185B1

反応ノート

読み込み中…