Acetic Anhydride → HCID 22614793、化合物
反応式
[NH2:1][C:2]1[C:9]([OH:10])=[C:8]([O:11][CH3:12])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[C:13](OC(=O)C)(=[O:15])[CH3:14]>N1C=CC=CC=1>[C:13]([NH:1][C:2]1[C:9]([OH:10])=[C:8]([O:11][CH3:12])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5])(=[O:15])[CH3:14]参加物
4
反応条件
- 温度
- 60 °C
実験手順
2-Amino-3-hydroxy-4-methoxybenzaldehyde (20.0 g, 0.12 mol) [M. Grossa, F. Wessely Monatsh. Chem. 1966, 97, 1384-1390] is dissolved at RT in a mixture of pyridine (250 ml) and acetic anhydride (250 ml). The solution is warmed to 60° C. and stirred for 1.5 h. The reaction solution is then poured onto a mixture of ice and half-concentrated aqueous NaCI solution (1:1), extracted with ethyl acetate (5 times), dried over MgSO4, filtered off and concentrated in vacuo. The title compound is obtained as a slightly yellow solid (12.5 g) after silica gel chromatography [petroleum ether/ethyl acetate (7:3)]. TLC, silica gel (glass plates), petroleum ether/ethyl acetate (7:3), Rf=0.23.