Acetic Acid → 5-bromo-7-methylquinazolin-4(3H)-one
反応式
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:12])[NH:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1.CO.CC(O)=O.[Br:19]Br>>[Br:19][C:4]1[CH:3]=[C:2]([CH3:1])[CH:11]=[C:10]2[C:5]=1[C:6](=[O:12])[NH:7][CH:8]=[N:9]2参加物
5
実験手順
To a solution of 7-methylquinazolin-4(3H)-one (900 mg, 5.63 mmol) in MeOH (180 mg, 5.63 mmol) and AcOH (5.07 g, 84.45 mmol) was added bromine (300 μL, 5.63 mmol) and the reaction mixture was stirred at rt for 4 h. Then the reaction mixture was quenched with an aq. solution of sodium thiosulphate. The precipitate obtained was filtered and dried to afford 900 mg of the title product. 1H NMR (300 MHz, DMSO-d6): δ 12.24 (br s, 1H), 8.18 (s, 1H), 8.08 (s, 1H), 7.66 (s, 1H), 2.48 (s, 3H).
後処理
- customThen the reaction mixture was quenched with an aq. solution of sodium thiosulphate
- customThe precipitate obtained
- filtrationwas filtered
- customdried
出典と根拠
- ORDレコード
- ord-bb17728b65a34f65a65c3a1a9155ae1a
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09006257B2
反応ノート
読み込み中…