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

HRID 719874

반응식

HRID 719874 반응식
[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

참가 물질

5

반응물 2

HCID 21897368N,N-dimethyl-6-nitropyridin-3-amineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 5743468N5,N5-Dimethylpyridine-2,5-diamine수율 94%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-39ea620acffd4fee9ee6ee05f850cc51
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132425B2

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