反应详情

A solution of 3.8 g (10.7 mmole) of 9-chloro-7-(2-chlorophenyl)-2-methyl-5H-pyrimido[5,4-d][2]benzazepine in 50 ml of acetic acid was hydrogenated at room temperature and atmospheric pressure in the presence of 0.5 g of prehydrogenated platinum oxide. After 3 hours about 500 ml (ca 2 equivalent) of hydrogen was absorbed and the catalyst was separated by filtration. The filtrate was concentrated at reduced pressure to dryness. The residue was dissolved in methylene chloride, washed with an excess of dilute ice cold sodium hydroxide, and dried over anhydrous sodium sulfate. The methylene chloride solution was diluted with an excess of methanolic hydrogen chloride and concentrated at reduced pressure. The residue was triturated with isopropanol and the crude product was collected by filtration. Recrystallization from methanol gave the pure product, m.p. 275°-276° C.

1. customwas hydrogenated at room temperature
2. customthe catalyst was separated by filtration
3. concentrationThe filtrate was concentrated at reduced pressure to dryness
4. dissolutionThe residue was dissolved in methylene chloride
5. washwashed with an excess of dilute ice cold sodium hydroxide
6. dry with materialdried over anhydrous sodium sulfate
7. additionThe methylene chloride solution was diluted with an excess of methanolic hydrogen chloride
8. concentrationconcentrated at reduced pressure
9. customThe residue was triturated with isopropanol
10. filtrationthe crude product was collected by filtration
11. customRecrystallization from methanol
12. customgave the pure product, m.p. 275°-276° C.