Formamidine acetate → 6-(N,N-Dimethylamino)-3H-pyrido[3,4-d]pyrimidin-4-one

HRID 2085939ノート

反応式

HRID 2085939 の反応式
[NH2:1][C:2]1[C:3]([C:11]([OH:13])=O)=[CH:4][C:5]([N:8]([CH3:10])[CH3:9])=[N:6][CH:7]=1.C(O)(=O)C.[CH:18](N)=[NH:19]>C(O)(=O)C>[CH3:10][N:8]([C:5]1[N:6]=[CH:7][C:2]2[N:1]=[CH:18][NH:19][C:11](=[O:13])[C:3]=2[CH:4]=1)[CH3:9]

参加物

4

反応物 2

HCID 160693Formamidine acetateHCID 227274305-Amino-2-(dimethylamino)isonicotinic acid

生成物 1

HCID 1358174466-(N,N-Dimethylamino)-3H-pyrido[3,4-d]pyrimidin-4-one収率 44.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

5-Amino-2-(N,N-dimethylamino)-pyridine-4-carboxylic acid (0.54 g) was treated with formamidine acetate (3.12 g) in glacial acetic acid (20 ml) and heated at reflux for 16 hours. The mixture was cooled, evaporated to dryness in vacuo and partitioned between ethyl acetate and water. The organic phase was separated, dried over magnesium sulphate and concentrated in vacuo to give, after chromatography on silica, the title compound (0.25 g); δH CDCl3 9.10(1H,d), 8.80(1H,s), 8.31(1H,s), 7.07(1H,s), 3.20(6H,s); m/z (M+1+) 191.

後処理

  1. temperatureheated
  2. temperatureat reflux for 16 hours
  3. temperatureThe mixture was cooled
  4. customevaporated to dryness in vacuo
  5. custompartitioned between ethyl acetate and water
  6. customThe organic phase was separated
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated in vacuo
  9. customto give

出典と根拠

ORDレコード
ord-1d9ef74bf37140eda579ef6d056235d9
出典データセット
uspto-grants-2004_04
特許番号
US06723726B1

反応ノート

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