Dimethyl Sulfoxide → HCID 136005593, compound

Participants

Reaction Conditions

Reaction Steps

Combine 2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride (351.6 mg, 1.32 mmol), (S)-2-[2-(2,4-difluoro-phenyl)-ethyl]-piperazine (600.0 mg, 2.65 mmol), N,N-diisopropylethylamine (171.0 mg, 1.32 mmol), DMSO (0.6 ml), and toluene (2.4 ml). Stir and heat the mixture at 105° C. After 48 hours, cool the mixture to ambient temperature and then dilute it with ethyl acetate and water. Remove the organic layer and wash it with 1N NaOH and brine. Dry (sodium sulfate) and concentrate the organic layer to residue. Purify the residue on silica gel using dichloromethane/methanol (95:5) to give 91.8 mg (16%) of the title compound as a brown foam: mp 69°, dec; mass spectrum (ion spray): m/z=439.0.

Provenance & Evidence