Thionyl Chloride → 4-Chloro-6-methoxy-7-nitroquinazoline hydrochloride
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[N+:13]([O-:15])=[O:14])[N:9]=[CH:8][NH:7][C:6]2=O.S(Cl)([Cl:19])=O>CN(C=O)C>[ClH:19].[Cl:19][C:6]1[C:5]2[C:10](=[CH:11][C:12]([N+:13]([O-:15])=[O:14])=[C:3]([O:2][CH3:1])[CH:4]=2)[N:9]=[CH:8][N:7]=1参加物
4
実験手順
A suspension of 6-methoxy-7-nitro-3,4-dihydroquinazolin-4-one (8 g, 36 mmol) in thionyl chloride (150 ml) and DMF (0.8 ml) was heated at reflux for 3 hours. Excess thionyl chloride was removed by evaporation and the residue azeotroped with toluene. The resulting solid was triturated with ether, collected by filtration and dried under vacuum to give 4-chloro-6-methoxy-7-nitroquinazoline hydrochloride(7.5 g, 75%).
後処理
- temperaturewas heated
- temperatureat reflux for 3 hours
- customExcess thionyl chloride was removed by evaporation
- customthe residue azeotroped with toluene
- customThe resulting solid was triturated with ether
- filtrationcollected by filtration
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-126788b0e06043449c8eb657bf59c5c6
- 出典データセット
- uspto-grants-2001_02
- 特許番号
- US06184225B2
反応ノート
読み込み中…