Sodium Carbonate → HCID 89923867, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 4-(tetrahydro-2H-pyran-4-yl)piperazine-1-carbonitrile (632 mg, 3.24 mmol), Ethanol (10 mL), hydroxylamine hydrochloric acid (257 mg, 3.70 mmol) and Na2CO3 (785 mg, 7.40 mmol) was heated to 80° C. After 1.5 h, the solids were filtered off and the filtrate concentrated in vacuo. The residue was dissolved into a minimum amount of methanol and treated with 5 mL of 1 M of HCl/Ether and diluted by acetone. Resulting solids were collected and dried in vacuo to afford the title compound (566 mg, 1.879 mmol, 76% yield) as white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm=11.88 (br. s., 4H), 11.20 (br. s., 1H), 10.17 (br. s., 1H), 8.26 (br. s., 2H), 4.09-3.87 (m, 5H), 3.69-3.49 (m, 4H), 3.42 (br. s., 1H), 3.26 (t, J=11.5 Hz, 2H), 3.17-2.98 (m, 2H), 2.00 (d, J=11.1 Hz, 2H), 1.83-1.64 (m, 2H); LC/MS (m/z) ES+ (ELSD)=229.2 (M+1).

Provenance & Evidence