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

HRID 2228597노트

반응식

HRID 2228597 반응식
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

참가 물질

4

반응물 3

HCID 3301EthylenediamineHCID 6342Acetonitrile2회HCID 184699642-Chloro-4-methyl-5-nitropyrimidine

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7936208f04e84b9db4d7fad817585762
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06417185B1

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