反应详情

To a solution of 2,2-dimethyl-4-oxo-4H-1,3-benzodioxine-6-carbonitrile (12 g, 0.06 mol) in methanol (500 mL) was added glacial acetic acid (3.5 g, 0.059 mol) and passed N2 for 30 min. To this was added Pd/C (2.4 g, 20%) and hydrogenated under 2 Bars of pressure for 22 h. The reaction mixture was filtered through celite and filtrate concentrated under vacuum. To the solid was added EtOAc (200 mL), stirred for 20 h and filtered. The solid was dried under vacuum to give 6-(aminomethyl)-2,2-dimethyl-4H-1,3-benzodioxin-4-one acetate (6 g, 38%). TLC:CHCl3/MeOH, 9:1, Rf: 0.15

1. customfor 30 min
2. filtrationThe reaction mixture was filtered through celite and filtrate
3. concentrationconcentrated under vacuum
4. additionTo the solid was added EtOAc (200 mL)
5. filtrationfiltered
6. customThe solid was dried under vacuum