Ammonia → HCID 76287210, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of methyl 2-[4-(2,4-dichlorophenyl)-1-methyl-3-(2-pyridyl)-6,7-dihydro-4H-pyrazolo[3,4-e][1,4]thiazepin-8-yl]acetate (0.350 g, 0.76 mmol, Preparation #12 step A), KCN (0.050 g, 0.77 mmol), and ammonia (10 mL, 7 M in MeOH, 70 mmol) in methanol (10 mL) was heated, in a sealed flask, for about 50 min at about 140° C. in a microwave. After cooling to rt the mixture was concentrated in vacuo. The residue was purified by column chromatography (SiO2, ethyl acetate/methanol 95:5) to give 2-[4-(2,4-dichlorophenyl)-1-methyl-3-(2-pyridyl)-6,7-dihydro-4H-pyrazolo[3,4-e][1,4]thiazepin-8-yl]acetamide (0.16 g, 0.36 mmol, 47%) as a beige solid: LC-MS (Table 1, Method b) Rt=5.49 min; m/z 448 (M+H)+.

Provenance & Evidence