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

HRID 566383ノート

反応式

HRID 566383 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-7f8ce20c188d414f818cf5e9796d00aa
出典データセット
uspto-grants-2001_01
特許番号
US06174889B1

反応ノート

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