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N-(2-methoxyphenyl)nicotinamide → HCID 13051663、化合物

HRID 2199052
ノート
印刷プレビュー

反応式

HRID 2199052 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 787042N-(2-methoxyphenyl)nicotinamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 13051663HCID 13051663、化合物収率 60%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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%

後処理

  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

出典と根拠

ORDレコード
ord-da4f3b872a5b4eb3a35c013ef0ebc88a
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04361572

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート