Diethyl Ether →
反応式
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]#[N:12])=[CH:6][C:5]=1[O:13][CH3:14])[CH3:2].[C:15](OC(=O)C)(=[O:17])[CH3:16].[Cl:22]([OH:26])(=[O:25])(=[O:24])=[O:23].[CH2:27]([O:29]CC)[CH3:28]>>[Cl:22]([O-:26])(=[O:25])(=[O:24])=[O:23].[C:15]([NH:12][C:11]1[O:29][CH2+:27]([CH3:28])[C:8]2[CH:9]=[C:4]([O:3][CH2:1][CH3:2])[C:5]([O:13][CH3:14])=[CH:6][C:7]=2[CH:10]=1)(=[O:17])[CH3:16]参加物
4
実験手順
To an ice-cooled and stirred solution of 25 grams 4-ethoxy-3-methoxyphenylacetonitrile (0.13 mmol) in 74 ml acetic anhydride (0.785 mol) was slowly added perchloric acid (70%, 11.7 N, 15.5 ml, 0.182 mol) over a 15 minute period. The dark reaction mixture slowly became a yellow slurry and was stirred at room temperature for 42 hours. The mixture was diluted with 200 ml diethyl ether and a crystalline yellow solid was isolated by filtration, washed with diethyl ether and dried in vacuo to provide 47.3 grams of Compound 8d (100% yield) having a melting point of 188°-189° C. (with decomposition).
後処理
- custom