Dimethylformamide → Ethyl 2-(4-cyanophenyl)-3-(dimethylamino)acrylate
反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1)#[N:2].[CH3:15][N:16]([CH:18]=O)[CH3:17]>>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9](=[CH:15][N:16]([CH3:18])[CH3:17])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1)#[N:2]参加物
3
実験手順
Combined ethyl 2-(4-cyanophenyl)acetate (25 g, 0.132 mol) with DMF-DEA (60 mL) and heated to 70° C. for 3 hours. The reaction mixture was cooled to room temperature and concentrated and then purified by flash chromatography to give the title compound (20 g, 62%) as a solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.71 (d, J=8.4 Hz, 2H), 7.59 (s, 1H), 7.29 (d, J=8.4 Hz, 2H), 4.03 (q, J=6.8 Hz, 2H), 2.67 (s, 6H), 1.13 (t, J=6.8 Hz, 3H).
後処理
- concentrationconcentrated
- custompurified by flash chromatography
出典と根拠
- ORDレコード
- ord-b0ce9e07dcc04befb7861bef45cb17f4
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040522B2
反応ノート
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