Ammonia → 3-Methylpyridine-2,6-diamine

HRID 910572

반응식

HRID 910572 반응식
[CH3:1][CH:2]([CH2:5][CH2:6][C:7]#[N:8])[C:3]#[N:4].[NH3:9]>[Pd]>[CH3:1][C:2]1[C:3]([NH2:9])=[N:4][C:7]([NH2:8])=[CH:6][CH:5]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 206862-Methylpentanedinitrile

생성물 1

HCID 1039073-Methylpyridine-2,6-diamine

시약·촉매·용매 1

HCID 23938Palladium촉매2회

반응 조건

온도
200 °C

실험 절차

2-Methylglutaronitrile was combined with Pd.C (5 mol % of 10 wt % Pd on carbon) in a 10 mL Hastelloy shaker autoclave to which liquid NH3 was added. The mixture was heated at 200° C. for 45 h. The mixture was cooled to ambient temperature and the excess NH3 removed by N2 purge. The crude mixture was suspended in 10 mL anhydrous methanol, the catalyst was removed by syringe filtration, and the crude reaction mixture was concentrated in vacuo. 2-Methylglutaronitrile conversion was 100% to give 0.02 mmol of 3-methylpyridine-2,6-diamine in 2.3% net yield.

후처리

  1. temperatureThe mixture was cooled to ambient temperature
  2. customthe excess NH3 removed by N2
  3. custompurge
  4. customthe catalyst was removed by syringe
  5. filtrationfiltration
  6. customthe crude reaction mixture
  7. concentrationwas concentrated in vacuo

출처 및 근거

ORD 기록
ord-7111e65421014e1b85ed2eaa4bf285da
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022167B2

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