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

HRID 606493노트

반응식

HRID 606493 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 22641269Acetate-hydrochloric acid용매

반응 조건

온도
80 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-e10b5da21dd94dfa8c525df5b61e8e3c
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915267B2

반응 노트

불러오는 중…