反应详情

In a sealed tube, 3.0 g of 1-chloromethyl-5,8-dimethoxyisochroman and 6.0 g of N-methylpiperazine were heated at 150°-160° C for 16 hours. After cooling, the reaction mixture was diluted with 200 ml of water and the oily precipitate was extracted with chloroform. The extract was rinsed with water, dried and concentrated under reduced pressure. The residue was chromatographed on a column of silica gel, elution being carried out with a solvent mixture of acetone, benzene and methanol (2:2:1). The oil thus obtained was converted to the fumarate and recrystallized from a solvent mixture of methanol and ether. By this procedure was obtained 1.3 g of 5,8-dimethoxy-1-(4-methylpiperazinyl)methylisochroman fumarate as pale-yellow needles, melting point: 188°-191° C.

1. temperatureAfter cooling
2. extractionthe oily precipitate was extracted with chloroform
3. washThe extract was rinsed with water
4. customdried
5. concentrationconcentrated under reduced pressure
6. customThe residue was chromatographed on a column of silica gel, elution
7. additionbeing carried out with a solvent mixture of acetone, benzene and methanol (2:2:1)
8. customThe oil thus obtained
9. customrecrystallized from a solvent mixture of methanol and ether