Potassium Carbonate → 3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carbaldehyde
反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[OH:14])[CH:9]=[O:10])=[O:4].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[O:4]=[C:3]1[NH:5][C:6]2[CH:7]=[C:8]([CH:9]=[O:10])[CH:11]=[CH:12][C:13]=2[O:14][CH2:2]1参加物
4
実験手順
3-(Chloroacetylamino)-4-hydroxy-benzaldehyde (2.4 g, 13.2 mmol) and potassium carbonate (9.1 g, 66.1 mmol) are stirred at room temperature in 50 mL of acetonitrile for 12 hours. The acetonitrile is evaporated and the residue is taken up in 50 mL of water. After standing at room temperature for 10 minutes, the precipitate is collected by filtration and recrystallized from ethyl acetate to give 1.4 g (60% yield) of 3-oxo-3,4-dihydro-2H-benzo[1,4]oxazine-6-carbaldehyde; mp 220-222° C.
後処理
- customThe acetonitrile is evaporated
- filtrationthe precipitate is collected by filtration
- customrecrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-7b53db98cf2f441ba191a2e606e1983f
- 出典データセット
- uspto-grants-2001_01
- 特許番号
- US06177422B1
反応ノート
読み込み中…