Ethyl cyanoformate → Ethyl 5,6-difluoro-4-oxo-3,4-dihydroquinazoline-2-carboxylate

HRID 606493ノート

反応式

HRID 606493 の反応式
Cl.[F:2][C:3]1[C:13]([F:14])=[C:7]([C:8]([O:10]CC)=O)[C:6]([NH2:15])=[CH:5][CH:4]=1.[C:16]([C:18]([O:20][CH2:21][CH3:22])=[O:19])#[N:17]>Cl.C(O)(=O)C>[F:14][C:13]1[C:3]([F:2])=[CH:4][CH:5]=[C:6]2[C:7]=1[C:8](=[O:10])[NH:17][C:16]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[N:15]2

参加物

4

反応物 2

HCID 69336Ethyl cyanoformateHCID 66768485Ethyl 6-amino-2,3-difluorobenzoate hydrochloride

生成物 1

HCID 136029322Ethyl 5,6-difluoro-4-oxo-3,4-dihydroquinazoline-2-carboxylate収率 82%

試薬・触媒・溶媒 1

HCID 22641269Acetate-hydrochloric acid溶媒

反応条件

温度
80 °C

実験手順

Ethyl 5,6-difluoroanthranilate hydrochloride (2.50 g, 10.5 mmol) was suspended in 1N hydrogen chloride-acetic acid solution (50 mL), ethyl cyanoformate (1.14 g, 11.6 mmol) was added thereto, and the mixture was stirred under heating at 80° C. for 3 hr. The reaction mixture allowed to cool to room temperature, and concentrated under reduced pressure. The residue was suspended in ethanol, and the insoluble material was collected by filtration to give the title compound as a white powder (2.18 g, 82%).

後処理

  1. temperatureto cool to room temperature
  2. concentrationconcentrated under reduced pressure
  3. filtrationthe insoluble material was collected by filtration

出典と根拠

ORDレコード
ord-e10b5da21dd94dfa8c525df5b61e8e3c
出典データセット
uspto-grants-2011_03
特許番号
US07915267B2

反応ノート

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