Nitrogen → 2-Acetamido-5-aminopyridine

HRID 865673

반응식

HRID 865673 반응식
N#N.[C:3]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][N:8]=1)(=[O:5])[CH3:4].C([O-])=O.[NH4+]>CN(C=O)C.[Pd].CO>[C:3]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][N:8]=1)(=[O:5])[CH3:4]

참가 물질

7

반응물 3

HCID 947NitrogenHCID 3451252-Acetamido-5-nitropyridineHCID 2723923Ammonium formate

생성물 1

HCID 27352192-Acetamido-5-aminopyridine수율 88.2%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 6228Dimethylformamide용매

실험 절차

A N2 covered solution of 1.19 g (6.6 mmol) of the product from Step 1 in 24 ml of DMF was treated with 2.07 g (32.9 mmol) of ammonium formate followed by 0.36 g of palladium on carbon catalyst. After stirring vigorously at room temperature for 17 hours, the reaction was diluted with MeOH and the catalyst was removed by filtration through celite. The filtrate was concentrated in vacuo and the residue was chromatographed over silica gel (3% MeOH: 0.3% NH4OH: CH2Cl2) to yield 0.876 g, m.p. 152°-153.5° C. (88.2%) of the titled product.

후처리

  1. customthe catalyst was removed by filtration through celite
  2. concentrationThe filtrate was concentrated in vacuo
  3. customthe residue was chromatographed over silica gel (3% MeOH: 0.3% NH4OH: CH2Cl2)

출처 및 근거

ORD 기록
ord-96c5e8a930fb438ebc8d061ffae6a959
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05567722

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