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N-(2-methoxyphenyl)nicotinamide → HCID 13051663, 화합물

HRID 2199052
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HRID 2199052 반응식
[C:1]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[H][H]>C(O)C.[Pd]>[C:1]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])(=[O:8])[C:2]1[CH2:7][CH2:6][CH2:5][NH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 787042N-(2-methoxyphenyl)nicotinamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 13051663HCID 13051663, 화합물수율 60%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Twenty-seven grams of N-nicotinoyl-2-methoxyaniline was dissolved in 800 ml of 10% hydrous ethanol. To the solution, 5 g of 10% palladium-on-carbon was added and the mixture was hydrogenated at 40° to 50° C. under atmospheric pressure. After 2 mols of hydrogen was introduced over a period of about 6 hours, the reaction was stopped and the catalyst was removed. The liquid reaction mixture was concentrated and the residual oil was purified with column chromatography on silica gel and recrystallized from hydrous methanol to give N-(1,4,5,6-tetrahydronicotinoyl)-2-methoxyaniline having a melting point of 126°-128° C. Yield=60%

후처리

  1. customwas hydrogenated at 40° to 50° C. under atmospheric pressure
  2. customthe catalyst was removed
  3. customThe liquid reaction mixture
  4. concentrationwas concentrated
  5. customthe residual oil was purified with column chromatography on silica gel
  6. customrecrystallized from hydrous methanol

출처 및 근거

ORD 기록
ord-da4f3b872a5b4eb3a35c013ef0ebc88a
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04361572

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