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

HRID 719874

反応式

HRID 719874 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.[H][H]>C(O)C.[Pd]>[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

5

反応物 2

HCID 21897368N,N-dimethyl-6-nitropyridin-3-amineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 5743468N5,N5-Dimethylpyridine-2,5-diamine収率 94%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of dimethyl-(6-nitro-pyridin-3-yl)-amine (0.64 g, 3.83 mmol) in ethanol (45 mL) was treated with 10% palladium on activated carbon (203 mg). The reaction mixture was stirred under a positive pressure of hydrogen gas (balloon) at 25° C. and atmospheric pressure overnight. The catalyst was then filtered off through a pad of celite, and the celite pad was washed well with ethanol. The filtrate was concentrated in vacuo to afford N5,N5-dimethyl-pyridine-2,5-diamine (493.6 mg, 94%) as a dark red-purple oil: EI-HRMS m/e calcd for C7H11N3 (M+) 137.0953, found 137.0957.

後処理

  1. customatmospheric pressure overnight
  2. filtrationThe catalyst was then filtered off through a pad of celite
  3. washthe celite pad was washed well with ethanol
  4. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-39ea620acffd4fee9ee6ee05f850cc51
出典データセット
uspto-grants-2006_11
特許番号
US07132425B2

関連ノート

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