Hydrochloric Acid → Ethyl 5-methyl-4-oxo-3,4-dihydroquinazoline-2-carboxylate

HRID 606495ノート

反応式

HRID 606495 の反応式
[NH2:1][C:2]([C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:5]=1[NH:11][C:12](=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:3].CC[O-].[Na+].Cl>C(O)C>[CH3:10][C:9]1[CH:8]=[CH:7][CH:6]=[C:5]2[C:4]=1[C:2](=[O:3])[NH:1][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:11]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 66768983Ethyl ((2-(aminocarbonyl)-3-methylphenyl)amino)(oxo)acetate

生成物 1

HCID 136029326Ethyl 5-methyl-4-oxo-3,4-dihydroquinazoline-2-carboxylate収率 64%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of ethyl ((2-(aminocarbonyl)-3-methylphenyl)amino)(oxo)acetate (760 mg, 3.04 mmol) in ethanol (15 mL) was added dropwise sodium ethylate (20% ethanol solution, 1.14 g, 3.34 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2 hr. 1N Hydrochloric acid (5 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was suspended in diisopropyl ether-ethanol, and the insoluble material was collected by filtration to give the title compound as a white powder (450 mg, 64%).

後処理

  1. temperaturecooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. filtrationthe insoluble material was collected by filtration

出典と根拠

ORDレコード
ord-5a3f68c73d6243ca89356bde917f3824
出典データセット
uspto-grants-2011_03
特許番号
US07915267B2

反応ノート

読み込み中…