反应详情

温度

125 °C

Benzoic anhydride (10.27 g) was added to a solution of 1-aminoisoquinolin-6-ol (3.312 g) in pyridine (53 ml) at ambient temperature. The mixture was heated at 125° C. for 1 h, the pyridine was removed under reduced pressure and excess pyridine was removed by azeotroping with toluene (X2). Water was added and the mixture extracted with dichloromethane (X3), dried (sodium sulphate) and concentrated in vacuo to give a solid precipitate. Recrystallisation with dichloromethane-diethyl ether gave benzoic acid 1-benzylaminoisoqinolin-6-yl ester (6 g), EIMS: m/z=369.1 [M+H]+.

1. customthe pyridine was removed under reduced pressure and excess pyridine
2. customwas removed
3. customby azeotroping with toluene (X2)
4. additionWater was added
5. extractionthe mixture extracted with dichloromethane (X3)
6. dry with materialdried (sodium sulphate)
7. concentrationconcentrated in vacuo
8. customto give a solid precipitate
9. customRecrystallisation with dichloromethane-diethyl ether