Phosphorus oxychloride → 4-Chloro-8-iodo-7-methylquinazoline
反応式
P(Cl)(Cl)([Cl:3])=O.[I:6][C:7]1[C:8]([CH3:18])=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][NH:13][C:12]2=O>>[Cl:3][C:12]1[C:11]2[C:16](=[C:7]([I:6])[C:8]([CH3:18])=[CH:9][CH:10]=2)[N:15]=[CH:14][N:13]=1参加物
3
実験手順
Phosphorous oxychloride (19.5 mL, 210 mmol) and 8-iodo-7-methylquinazolin-4(3H)-one (2.00 g, 6.99 mmol) were added to a round bottomed flask. The reaction mixture was heated at reflux for 2 h. Upon cooling, excess POCl3 was removed under reduced pressure and the remaining crude product dissolved in DCM (100 mL) and washed with ice-cold water (300 mL) to remove excess acid. The crude residue dissolved in DCM was then dried over anhydrous sodium sulfate and concentrated in vacuo to give 4-chloro-8-iodo-7-methylquinazoline (1.96 g, 92%) as an amorphous brown solid. MS (M+H)+ 305.
後処理
- temperatureThe reaction mixture was heated
- temperatureat reflux for 2 h
- temperatureUpon cooling
- customexcess POCl3 was removed under reduced pressure
- dissolutionthe remaining crude product dissolved in DCM (100 mL)
- washwashed with ice-cold water (300 mL)
- customto remove excess acid
- dissolutionThe crude residue dissolved in DCM
- dry with materialwas then dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-5431aab719d340fea363d8eb6c42cf1c
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07989461B2
反応ノート
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