Nitric Acid → HCID 22008421, compound

Participants

Reaction Steps

5.0 g 5-(2-fluorophenyl)-7-hydroxy-3-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine was dissolved in 90 ml of a mixture of acetic acid and cooled in ice-water bath 0° C. Under stirring was added 1.7 ml fuming nitric acid and the mixture was stirred in the cold for 1 h. The reaction mixture was neutralized (pH 7.9) and the precipitate was extracted with ethyl acetate, dried and evaporated. After column chromatography (kieselgel/CH2Cl2: CH3OH 95:5) was isolated yellow crystals. M.p. 90-94° C. (dec). NMR: C5H 4.61 d; C6H g 41% 6 s and C9H 7.88 s ppm. respectively.

Provenance & Evidence