Phosphorus oxychloride → 1-Chloro-2,7-naphthyridine
反応式
O[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[N:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[N:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1参加物
3
反応条件
- 温度
- 130 °C
実験手順
A pressure bottle, equipped with a magnetic stirrer, was charged with 1-hydroxy-2,7-naphthyridine (2.6 g, 17.8 mmol) and 100 mL of phosphorous oxychloride. The bottle was sealed and heated at 130° C. overnight. Upon cooling, the bottle was opened and the excess POCl3 was removed by evaporation in vacuo. The residue was treated with excess saturated Na2CO3 and extracted twice with CHCl3. The organic layer was washed with brine and dried (Na2SO4). Evaporation of the solvent afforded the product as a light brown solid (2.0 g, 68%, purity 90-95% based on NMR). The product was of suitable purity for use in the next step.
後処理
- customA pressure bottle, equipped with a magnetic stirrer
- customThe bottle was sealed
- temperatureUpon cooling
- customthe excess POCl3 was removed by evaporation in vacuo
- additionThe residue was treated with excess saturated Na2CO3
- extractionextracted twice with CHCl3
- washThe organic layer was washed with brine
- dry with materialdried (Na2SO4)
- customEvaporation of the solvent
出典と根拠
- ORDレコード
- ord-5ffb66c59a6d4d5482ea0ed95b2d6815
- 出典データセット
- uspto-grants-1989_08
- 特許番号
- US04859671
反応ノート
読み込み中…