Hydrochloric Acid → 7-Bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid

In 1N sodium hydroxide (13.0 ml) and THF:ethanol (1:1, 50 ml) was dissolved ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate (2.77 g), and the mixture was stirred at room temperature for 15 hours. To the mixture was added 1N hydrochloric acid (12.5 ml), and the mixture was concentrated. To the residue was added water (200 ml), and the mixture was adjusted to pH 2 with 1N hydrochloric acid. The mixture was extracted with ethyl acetate(300 ml×3), and the organic layer was dried with magnesium sulfate. The solvent was evaporated under reduced pressure to give 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid (2.52 g, 100%).

1. concentrationthe mixture was concentrated
2. additionTo the residue was added water (200 ml)
3. extractionThe mixture was extracted with ethyl acetate(300 ml×3)
4. dry with materialthe organic layer was dried with magnesium sulfate
5. customThe solvent was evaporated under reduced pressure

ORD-Eintrag

ord-43915a424f4345c4b4584769d254a322

Quelldatensatz

uspto-grants-2001_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06172061B2