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

HRID 641714노트

반응식

HRID 641714 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-21c186dee0fe4c17b3201d03ee672785
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696214B2

반응 노트

불러오는 중…