Phosphorus oxychloride → 4-Chloro-3-(2-chloroethyl)cinnoline
反応式
[Cl:1][CH2:2][CH2:3][C:4]1[C:13](=O)[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][N:5]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:1][CH2:2][CH2:3][C:4]1[N:5]=[N:6][C:7]2[C:12]([C:13]=1[Cl:17])=[CH:11][CH:10]=[CH:9][CH:8]=2参加物
3
実験手順
3-(2-Chloroethyl)-4-oxo-(1H)-cinnoline (9 g, 0.043 mol) and phosphorus oxychloride (90 ml) were heated under reflux for 1 hour. After allowing to cool, the excess phosphorus oxychloride was evaporated under reduced pressure and the residue was poured onto ice (100 g), basified with concentrated ammonia solution, and extracted with chloroform (3×100 ml). The chloroform extracts were combined, dried over magnesium sulphate and evaporated under reduced pressure to give a solid, 8.00 g. Recrystallization from diethyl ether gave the title compound, m.p. 81-82°.
後処理
- temperatureunder reflux for 1 hour
- temperatureto cool
- customthe excess phosphorus oxychloride was evaporated under reduced pressure
- additionthe residue was poured onto ice (100 g)
- extractionextracted with chloroform (3×100 ml)
- dry with materialdried over magnesium sulphate
- customevaporated under reduced pressure
- customto give a solid, 8.00 g
- customRecrystallization from diethyl ether
出典と根拠
- ORDレコード
- ord-d075416f26954eb8b0f827581e8b9a58
- 出典データセット
- uspto-grants-1991_01
- 特許番号
- US04988695
反応ノート
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