Perchloric Acid →
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].[Cl:15]([OH:19])(=[O:18])(=[O:17])=[O:16]>CC(OCC1C2C(=CC=CC=2)C(COC(C)=O)=C2C=1C=CC=C2)=O.C(OCC)C>[Cl:15]([O-:19])(=[O:18])(=[O:17])=[O:16].[C:1]([NH:12][C:11]1[O:13][CH2+:5]([CH3:4])[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:3])[CH3:2]参加物
4
実験手順
To an ice-cooled and stirred soluton of 25 grams 4-ethoxy-3-methoxyphenylacetonitrile (0.13 mmol) in 74 ml acetic ahnydride (0.785 mol) was slowly added perchloric acid (70%, 11.7N, 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 product (100% yield) having a melting point of 188°-189° C. (with decomposition).