反应详情

温度

45 °C

150 g of polyphosphoric acid (Acros) was added to a mixture of 1,2,3-trimethoxybenzene (10.0 g, 59.47 mmol), and mono-methyl adipate (13.04 mL g, 89.20 mmol) in a 250 mL round bottom flask equipped with a mechanical stirrer. The reaction mixture was stirred for 2.5 h at 45° C. The reaction mixture was then poured into a 1000 mL beaker containing around 500 mL of ice, and stirred well. Tan colored product precipitated out which was then filtered and washed with water and dried under vacuum. 17.18 g (93%) of 65 was obtained, which was pure by NMR. Rf: 0.42 (40:60 EtOAc:Hexanes)

1. customequipped with a mechanical stirrer
2. additionThe reaction mixture was then poured into a 1000 mL beaker
3. stirringstirred well
4. customTan colored product precipitated out which
5. filtrationwas then filtered
6. washwashed with water
7. customdried under vacuum