Dimethylformamide diethylacetal → Ethyl 3-(dimethylamino)-2-(5-bromopyridin-3-yl)acrylate
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[N:6][CH:7]=1.C(O[CH:17](OCC)[N:18]([CH3:20])[CH3:19])C>>[CH3:17][N:18]([CH3:20])[CH:19]=[C:8]([C:4]1[CH:5]=[N:6][CH:7]=[C:2]([Br:1])[CH:3]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10]参加物
3
実験手順
5.1 g (20.9 mmol) of the compound from Example 10A are stirred in 7.2 ml (6.2 g, 41.8 mmol) of dimethylformamide diethyl acetal at a bath temperature of 100° C. for 16 h. After cooling, the mixture is concentrated under reduced pressure, the residue is stirred in diisopropyl ether, and the solid is filtered off and finally washed with diisopropyl ether. The crude product is dried under reduced pressure for 16 h.
後処理
- temperatureAfter cooling
- concentrationthe mixture is concentrated under reduced pressure
- filtrationthe solid is filtered off
- washfinally washed with diisopropyl ether
- dry with materialThe crude product is dried under reduced pressure for 16 h.
出典と根拠
- ORDレコード
- ord-fdad1c24727e4b5282819bcce813ea66
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524699B2
反応ノート
読み込み中…