Formamidine acetate → HCID 178487763、化合物
反応式
[NH2:1][C:2]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].C(O)(=O)C.[CH:17](N)=[NH:18]>COCCO>[CH3:12][O:11][C:9]1[CH:10]=[C:2]2[C:3]([C:4]([OH:5])=[N:18][CH:17]=[N:1]2)=[CH:7][CH:8]=1参加物
4
反応条件
- 温度
- 130 °C
実験手順
Step 1 A mixture of 2-amino-4-methoxybenzoic acid (0.5 g, 2.99 mmol) and formamidine acetate (0.623 g, 5.98 mmol) in 2-methoxyethanol (4 mL) was heated at 130° C. After 15.25 h, the mixture was cooled to rt. The resulting precipitate was collected by filtration, washed with methanol and dried to provide 7-methoxyquinazolin-4-ol as a tan solid (473 mg, 90%). 1H NMR (400 MHz, DMSO-d6) δ 12.08 (1 H, br. s.), 8.06 (1 H, s), 8.03 (1 H, d, J=9.5 Hz), 7.03-7.14 (2 H, m), 3.90 (3 H, s).
後処理
- temperaturethe mixture was cooled to rt
- filtrationThe resulting precipitate was collected by filtration
- washwashed with methanol
- customdried
出典と根拠
- ORDレコード
- ord-dbb7e3abeda4448e845102690cab76c6
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08362065B2
反応ノート
読み込み中…