Formamidine acetate → 5,7-dimethoxyquinazolin-4(3H)-one

HRID 641714ノート

反応式

HRID 641714 の反応式
[NH2:1][C:2]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[C:8]([O:14][CH3:15])[C:3]=1[C:4](OC)=[O:5].C(O)(=O)C.[CH:20](N)=[NH:21]>COCCO>[CH3:15][O:14][C:8]1[CH:9]=[C:10]([O:12][CH3:13])[CH:11]=[C:2]2[C:3]=1[C:4](=[O:5])[NH:21][CH:20]=[N:1]2

参加物

4

反応物 2

HCID 160693Formamidine acetateHCID 11550253Methyl 2-amino-4,6-dimethoxybenzoate

生成物 1

HCID 1355106675,7-dimethoxyquinazolin-4(3H)-one収率 92.8%

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

A mixture of methyl 2-amino-4,6-dimethoxybenzoate (16 g), formamidine acetate (24 g) and 2-methoxyethanol (330 ml) was stirred and heated to reflux until all of the starting material had reacted. The mixture was evaporated and the residue was triturated under water (100 ml). The resultant solid was isolated, washed with water and dried under vacuum to give 5,7-dimethoxy-3,4-dihydroquinazolin-4-one (14.5 g); NMR Spectrum: (DMSOd6) 3.82 (s, 3H), 3.86 (s, 3H), 6.5 (s, 1H), 6.7 (s, 1H), 7.9 (s, 1H), 11.7 (br s, 1).

後処理

  1. temperatureheated
  2. temperatureto reflux until all of the starting material
  3. customhad reacted
  4. customThe mixture was evaporated
  5. customthe residue was triturated under water (100 ml)
  6. customThe resultant solid was isolated
  7. washwashed with water
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-21c186dee0fe4c17b3201d03ee672785
出典データセット
uspto-grants-2010_04
特許番号
US07696214B2

反応ノート

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