Hydrochloric Acid → HCID 13225522, compound

To 20 ml of dimethylmalonate was added 1.9 g (16.8 mmol) of potassium tertiary butoxide with stirring under nitrogen, and after 15 min, 2.0 g (5.59 mmol) of 2,9-dichloro-7-(2-fluorophenyl)-5H-pyrimido[5,4-d][2]benzazepine was added. The reaction was kept at 110° C. for 2 hr and 140° C. for 4 hr. Ice was added to the reaction mixture which was then acidified with concentrated hydrochloric acid, and extracted with 100 ml of ether. The ether layer was extracted with 25 ml of 3N hydrochloric acid, and the combined acid layers were made basic with ammonium hydroxide and extracted with ether (2×100 ml). The solution was dried, charcoal filtered and concentrated to a small volume. Petroleum ether was added and the product was filtered and recrystallized from the same solvents to give white rods, mp 98°-103° C.

1. waitThe reaction was kept at 110° C. for 2 hr and 140° C. for 4 hr
2. additionIce was added to the reaction mixture which
3. extractionextracted with 100 ml of ether
4. extractionThe ether layer was extracted with 25 ml of 3N hydrochloric acid
5. extractionextracted with ether (2×100 ml)
6. customThe solution was dried
7. filtrationcharcoal filtered
8. concentrationconcentrated to a small volume
9. additionPetroleum ether was added
10. filtrationthe product was filtered
11. customrecrystallized from the same solvents
12. customto give white rods, mp 98°-103° C.

ORD record

ord-87051f543bcd4d78921eda70986f29d6

Source dataset

uspto-grants-1984_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04481142