Phosphorus oxychloride → 2-Chloro-4-(2-chlorophenyl)-6-nitroquinazoline
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([N+:18]([O-:20])=[O:19])[CH:16]=2)[NH:11][C:10](=O)[N:9]=1.P(Cl)(Cl)([Cl:24])=O>>[Cl:24][C:10]1[N:9]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([N+:18]([O-:20])=[O:19])[CH:16]=2)[N:11]=1参加物
3
実験手順
A mixture of 40 g of 4-(2-chloro phenyl) 6-nitro 2-quinazolone are 600 ml of phosphorus oxychloride is heated to reflux for 4 hours. The phosphorus oxychloride is evaporated in vacuo to dryness, then the residue is poured into an ice-water mixture. It is rendered alkaline with a 10% sodium hydroxide solution. The precipitate is drained and washed with acetonitrile. The product is purified by chromatography over a column of silica. By eluting with a chloroform-methanol (95-5 vol/vol) mixture, the expected product is isolated. Weight: 27 g; m.p.: 228° C. (isopropanol).
後処理
- temperatureis heated
- temperatureto reflux for 4 hours
- customThe phosphorus oxychloride is evaporated in vacuo to dryness