Malonic Acid → 2,4,8-Trichloro-7-methoxyquinoline
反応式
[ClH:1].[Cl:2][C:3]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[CH:6][C:4]=1[NH2:5].[C:12](O)(=O)[CH2:13][C:14](O)=O.O(Cl)[Cl:20].[P]>O>[Cl:1][C:14]1[CH:13]=[C:12]([Cl:20])[C:6]2[C:4](=[C:3]([Cl:2])[C:9]([O:10][CH3:11])=[CH:8][CH:7]=2)[N:5]=1参加物
5
実験手順
A mixture of 2-chloro-3-methoxyaniline hydrochloride 215d (15 g, 1 eq.), malonic acid (12.06 g, 1.5 eq.), and phosphorus oxochloride (80 mL) was refluxed for 16 hrs. The reaction mixture was slowly poured into water and extracted with DCM. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude material was purified on silica pad, eluted with DCM, to yield compound 220d as a white solid in 74% yield.
後処理
- temperaturewas refluxed for 16 hrs
- extractionextracted with DCM
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude material was purified on silica pad
- washeluted with DCM
出典と根拠
- ORDレコード
- ord-964eb2fc958e476b84c7e6dd05937534
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09284307B2
反応ノート
読み込み中…