Triethylamine → HCID 58714287, compound

Participants

Reaction Steps

A solution of 7-Acetyl-3-(S)-(4-chloro-phenyl)-4-[1-(R)-(4-chloro-phenyl)-ethyl]-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione (50 mg, 0.11 mmol), hydroxylamine hydrochloride salt (22 mg, 0.33 mmol), triethylamine (0.074 mL, 0.55 mmol) in EtOH (0.5 mL) was heated to 80° C. After 2 h reaction solution was applied to a prep tlc plate (Analtech Silica Gel GF, 20×20 cm, 2000 microns) and developed using methylene chloride/MeOH 10:1. Desired bands were scraped off, extracted with MeOH, filtered and concentrated to give the title compound (2.4 mg). 1H NMR (400 MHz, DMSO-d6) δ 7.82–7.83 (m, 1H), 7.47–7.51 (m, 3H), 7.32 (s, 3H), 7.26–7.30 (m, 2H), 6.80–6.84 (m, 2H), 6.66–6.70 (d, J=8.4 Hz, 2H), 6.52–6.55 (d, J=8.6 Hz, 2H), 6.36–6.42 (m, 2H), 5.17 (s, 1H), 1.67–1.71 (d, J=7.3 Hz, 3H). Mass spectrum (LCMS, ESI pos.): Calcd for C25H21Cl2N3O3: 481.1; found 482.1 (M+H).

Provenance & Evidence