Sodium Hydroxide → HCID 9811366, compound

Participants

Reaction Steps

Triethylamine (1.34 ml) was added dropwise to a suspension of 4-amino-1-(3-phenylpropyl)piperidine dihydrochloride (1.40 g) and dimethylformamide (10 ml). Into the mixture which was stirred for 10 minutes, 5-thia-1,8b-diazaacenaphthylene-4-carboxylic acid (1.00 g) and diethyl cyanophosphonate (0.81 ml) were added. The mixture was stirred for 1 hour at room temperature, and 2 hours at 55° C. Ethyl acetate:tetrahydrofuran=4:1 (1.75 ml) and 1N-sodium hydroxide (30 ml) were added into the reaction mixture. The organic layer which was washed with sodium hydroxide (30 ml×3) and water (30 ml×2) was concentrated. The residual crystal which was added acetate (4 ml) was stirred for 1 hour at room temperature. This was dried under reduced pressure to obtain N-[1-(3-phenylpropan-1-yl)piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide (1.07 g, 63.6%).

Provenance & Evidence