N,N-dimethyl-6-nitropyridin-3-amine → N5,N5-Dimethylpyridine-2,5-diamine

HRID 600636

反応式

HRID 600636 の反応式
[CH3:1][N:2]([CH3:12])[C:3]1[CH:4]=[N:5][C:6]([N+:9]([O-])=O)=[CH:7][CH:8]=1>C(O)C>[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[N:5][CH:4]=1

参加物

3

反応物 1

HCID 21897368N,N-dimethyl-6-nitropyridin-3-amine

生成物 1

HCID 5743468N5,N5-Dimethylpyridine-2,5-diamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The N,N-dimethyl-6-nitropyridine-3-amine obtained above is taken up in 25 mL of ethanol. After addition of 4.8 g of stannous chloride, the reaction mixture is refluxed for 30 minutes and then concentrated to dryness. The residue is chromatographed on a column of silica, eluting with a 90/10 mixture of dichloromethane and ammoniacal methanol. The fractions containing the expected product are combined and concentrated to give 750 mg of 5-dimethylaminopyridine-2-amine in the form of a pasty yellow solid.

後処理

  1. temperaturethe reaction mixture is refluxed for 30 minutes
  2. concentrationconcentrated to dryness
  3. customThe residue is chromatographed on a column of silica
  4. washeluting with a 90/10 mixture of dichloromethane and ammoniacal methanol
  5. additionThe fractions containing the expected product
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-443e1c65d15a4ce9ba78985ffe739718
出典データセット
uspto-grants-2011_03
特許番号
US07902219B2

関連ノート

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