Diethyl (2,6-dichloronicotinoyl)-malonate → Ethyl 3-(2,6-dichloropyridin-3-YL)-3-oxopropanoate
反応式
[Cl:1][C:2]1[N:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:3]=1[C:4]([CH:6](C(OCC)=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]>O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[Cl:1][C:2]1[N:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]参加物
4
実験手順
The crude diethyl (2,6-dichloronicotinoyl)-malonate is refluxed for 2 hours in 45 ml of water and 90 mg of p-toluenesulphonic acid. The mixture is extracted using methylene chloride, and the methylene chloride phase is washed with water, dried over sodium sulphate and concentrated in vacuo. The crude product is purified on silica gel (eluent dichloromethane).
後処理
- extractionThe mixture is extracted
- washthe methylene chloride phase is washed with water
- dry with materialdried over sodium sulphate
- concentrationconcentrated in vacuo
- customThe crude product is purified on silica gel (eluent dichloromethane)
出典と根拠
- ORDレコード
- ord-96f345fc899f476b8d89da6f2a51e32d
- 出典データセット
- uspto-grants-1995_10
- 特許番号
- US05457104
反応ノート
読み込み中…