反应详情

温度

90 °C

Compound of example 117 (19.0 g, 92 mmol) was added to a solution of 1,3,5-trimethoxybenzene (21.8 g, 130 mmol) in glacial acetic acid (50 mL) at 25° C. HCl gas was bubbled through the reaction mixture for 1 h, slowly raising the temperature up to 90° C. Acetic acid was removed under reduced pressure and the semisolid residue was poured over crushed ice (300 g). The resulting solution was made basic using an aqueous 50% NaOH solution. The precipitated solid was filtered, washed with water and dried. The solid was added slowly to boiling methanol, stirred for fifteen minutes and filtered to remove traces of trimethoxybenzene and the filtrate was concentrated to get the title compound.

1. customHCl gas was bubbled through the reaction mixture for 1 h
2. customAcetic acid was removed under reduced pressure
3. additionthe semisolid residue was poured
4. customover crushed ice (300 g)
5. filtrationThe precipitated solid was filtered
6. washwashed with water
7. customdried
8. additionThe solid was added slowly
9. filtrationfiltered
10. customto remove traces of trimethoxybenzene
11. concentrationthe filtrate was concentrated