Hydrogen Peroxide → 2-(2-methoxy-6-methyl-phenyl)-7-methyl-3H-quinazolin-4-one
반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH3:9])=[CH:5][C:4]=1[NH:10][C:11](=O)[C:12]1[C:17]([CH3:18])=[CH:16][CH:15]=[CH:14][C:13]=1[O:19][CH3:20])#[N:2].[OH-:22].[Na+].OO>CCO>[CH3:20][O:19][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]([CH3:18])[C:12]=1[C:11]1[NH:2][C:1](=[O:22])[C:3]2[C:4](=[CH:5][C:6]([CH3:9])=[CH:7][CH:8]=2)[N:10]=1참가 물질
실험 절차
N-(2-Cyano-5-methyl-phenyl)-2-methoxy-6-methyl-benzamide (25 g, 0.09 mol) was suspended in 500 mL EtOH, and 121.3 g of 33% aq. NaOH (1 mol, 11 equiv) was added. To this was added a 35% H2O2 solution (50 mL, 0.58 mol), and the reaction was heated to reflux. Additional H2O2 was added dropwise until the reaction mixture became clear. EtOH was removed under reduced pressure, and the precipitate formed was removed by filtration. The solution was acidified with acetic acid to pH 5, and the precipitate formed was collected by filtration. The precipitate was washed twice with water and once with diethyl ether. The product was purified over alumina using EtOAc/heptane (1:1) as an eluent. Another purification was performed, over silica gel with the same eluent to yield 2-(2-methoxy-6-methyl-phenyl)-7-methyl-3H-quinazolin-4-one (1.61 g).
후처리
- temperaturethe reaction was heated to reflux
- customEtOH was removed under reduced pressure
- customthe precipitate formed
- customwas removed by filtration
- customthe precipitate formed
- filtrationwas collected by filtration
- washThe precipitate was washed twice with water and once with diethyl ether
- customThe product was purified over alumina
- customAnother purification
출처 및 근거
- ORD 기록
- ord-fdd2cb17eabb4fb8b6ac865230787d4c
- 출처 데이터셋
- uspto-grants-2012_10
- 특허 번호
- US08283354B2
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