Dimethylformamide diethylacetal → 3-(Dimethylamino)-2-(2-methylpyridin-3-yl)-acrylic acid ethyl ester
反応式
[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]1[C:7]([CH3:12])=[N:8][CH:9]=[CH:10][CH:11]=1)[CH3:2].C(O[CH:17](OCC)[N:18]([CH3:20])[CH3:19])C>>[CH2:1]([O:3][C:4](=[O:13])[C:5]([C:6]1[C:7]([CH3:12])=[N:8][CH:9]=[CH:10][CH:11]=1)=[CH:17][N:18]([CH3:20])[CH3:19])[CH3:2]参加物
3
実験手順
600 mg (3.35 mmol) of the compound from Example 39A are heated in 1.7 ml (10.0 mmol) dimethylformamide diethyl acetal overnight at 100° C. After cooling, the mixture is concentrated and the residue is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient).
後処理
- temperatureAfter cooling
- concentrationthe mixture is concentrated
- customthe residue is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient)
出典と根拠
- ORDレコード
- ord-cb97c7e2d28c4658968b7b1e75225c9f
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09085572B2
反応ノート
読み込み中…