Phosphorus oxychloride → 4-Chloro-6-iodo-2-(trifluoromethyl)quinazoline
反応式
[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[NH:6][C:5]2=O.O=P(Cl)(Cl)[Cl:19]>>[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[N:6]=[C:5]2[Cl:19]参加物
3
実験手順
6-iodo-2-trifluoromethyl-3H-quinazolin-4-one (3.1 g, 9.1 mmole) was mixed with 20 mL of POCl3, heated to reflux for 3 h, removed most of unreacted POCl3 under vacuo. The residue was extracted with 15 mL of NaHCO3 (sat) and 200 mL of ether, ether layer was dried with MgSO4 and concentrated to give the light yellow solid 3.05 g, mp 145°-146° C., MS (CI): m/z 359 (MH)+.
後処理
- temperatureheated
- temperatureto reflux for 3 h
- customremoved most of unreacted POCl3 under vacuo
- extractionThe residue was extracted with 15 mL of NaHCO3 (sat) and 200 mL of ether, ether layer
- dry with materialwas dried with MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1c2c0e41765540e09c1d2ad3da6ceec5
- 出典データセット
- uspto-grants-1997_08
- 特許番号
- US05658902
反応ノート
読み込み中…