HCID 14042135, 화합물 → HCID 70097075, 화합물

HRID 467629노트

반응식

HRID 467629 반응식
[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][CH:8]=[C:7]([C:12]2[CH:16]=[CH:15][O:14][CH:13]=2)[N:6]=1)=[O:4]>CO.[Pd]>[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][CH:8]=[C:7]([CH:12]2[CH2:16][CH2:15][O:14][CH2:13]2)[N:6]=1)=[O:4]

참가 물질

4

반응물 1

HCID 14042135HCID 14042135, 화합물

생성물 1

HCID 70097075HCID 70097075, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매2회HCID 887Methanol용매

실험 절차

A solution of 3-amino-6-(furan-3-yl)-pyrazine-2-carboxylic acid methyl ester (2.9 g, 13.2 mmol) in MeOH (150 ml) was treated with palladium on carbon (10%; 0.6 g, 0.28 mmol) and hydrogenated at 1.2 atmospheres for 40 h. Another 2 equivalents of palladium on carbon were consecutively added and the hydrogenation was continued for another 72 h. The reaction mixture was filtered and the catalyst was washed with MeOH. The solution was concentrated in vacuo and the product was obtained after purification by silica gel chromatography using a heptane/ethyl acetate gradient as light yellow solid (0.3 g, 10%).

후처리

  1. waitthe hydrogenation was continued for another 72 h
  2. filtrationThe reaction mixture was filtered
  3. washthe catalyst was washed with MeOH
  4. concentrationThe solution was concentrated in vacuo
  5. customthe product was obtained
  6. customafter purification by silica gel chromatography

출처 및 근거

ORD 기록
ord-43a9a55365c04b259751073af897ba2a
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623866B2

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