Dichloromethane methanol → HCID 137194527, compound

Participants

Reaction Steps

Combine 2-isopropyl-2,4-dihydro-1,2,3,4,9-pentaaza-benzo[f]azulen-10-ylamine (0.863 g, 3.56 mmol), (S)-2-phenethyl-piperazine (0.678 g, 3.56 mmol) in NMP (6.0 mL) and heat at 200° C. for 3 hours. Cool to ambient temperature and dilute with water (75 mL). Extract with ethyl acetate to give 1.59 g of the crude product. Silica gel chromatography, eluding with methylene chloride:methanol (100:7.5), to give the title compound as the free base. The dihydrochloride salt precipitates in ethyl acetate as a yellow solid: mp 210° C.; mass spectrum (ion spray): m/z=416 (M+1); Analysis for C24H31Cl2N7(0.5 H2O): calcd: C, 57.95; H, 6.48; N, 19.71; found: C, 58.01; H, 6.22; N, 19.70.

Provenance & Evidence