2-Amino-6-chloropyridine-3,5-dicarbonitrile → 2-Aminopyridine-3,5-dicarbonitrile

HRID 842705

반응식

HRID 842705 반응식
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[C:4](Cl)[N:3]=1>[Pd].O1CCOCC1>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[CH:4][N:3]=1

참가 물질

4

반응물 1

HCID 2959012-Amino-6-chloropyridine-3,5-dicarbonitrile

생성물 1

HCID 2959122-Aminopyridine-3,5-dicarbonitrile

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 312751,4-Dioxane용매

실험 절차

A mixture of 2-amino-6-chloro-3,5-dicyanopyridine (Synth. Comm. 1993, 2605, 15.0 g, 84 mmol) and 10% palladium on carbon (10.0 g) in dioxane (150 mL) was shaken on a Parr apparatus under hydrogen (55 psi) for 16 h. More catalyst (7.5 g) was added and after a further 4 h the reaction mixture was filtered through celite washing through with ethanol and evaporated in vacuo. The residue was partitioned between methylene chloride and 1 M HCl. The insoluble material was collected by filtration and dried to give the title compound. The methylene chloride layer was washed with brine, dried (Na2SO4) and evaporated in vacuo to give additional product:

후처리

  1. filtrationwas filtered through celite
  2. washwashing through with ethanol
  3. customevaporated in vacuo
  4. customThe residue was partitioned between methylene chloride and 1 M HCl
  5. filtrationThe insoluble material was collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-a57ce74854b24acfbc7930dae628fd29
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06376499B1

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