HCID 1211386、化合物 → Pyrido(2,3-b)(1,5)benzoxazepin-5(6H)-one
反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]([C:11]1[C:12](Cl)=[N:13][CH:14]=[CH:15][CH:16]=1)=[O:10].C[O-].[Na+]>CN(C)C=O>[N:13]1[C:12]2[O:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=3[NH:8][C:9](=[O:10])[C:11]=2[CH:16]=[CH:15][CH:14]=1参加物
4
実験手順
A mixture of 13.0 g of N-(2-hydroxyphenyl)-2-chloro-3-pyridinecarboxamide and 2.82 g of sodium methoxide in 100 ml of N,N-dimethylformamide is refluxed under argon for 3 hours. Sodium methoxide (0.50 g) is added and the mixture refluxed 2 hours and then stirred at room temperature for 2 days. The solvent is removed under high vacuum and the red-brown residue triturated with cold methanol. The mixture is filtered and the solid washed with chilled methanol to give 5.0 g of white solid, m.p. 250°-253° C.
後処理
- temperatureis refluxed under argon for 3 hours
- temperaturethe mixture refluxed 2 hours
- customThe solvent is removed under high vacuum
- customthe red-brown residue triturated with cold methanol
- filtrationThe mixture is filtered
- washthe solid washed with chilled methanol
出典と根拠
- ORDレコード
- ord-88bd20deb2ac4a0bba13a3d5e871b963
- 出典データセット
- uspto-grants-1998_12
- 特許番号
- US05849735
反応ノート
読み込み中…