Dimethylformamide → HCID 21708626, compound

Participants

Reaction Conditions

Reaction Steps

To DMF (50 ml, 0.68 mol) was slowly added POCl3 (50 ml, 0.54 mol) at 0° C. over 1 h. 1-Azabicyclo[3.3.1]nonane-4-one hydrochloride (17.5 g, 0.1 mol) was added in one portion and the reaction mixture heated at 100° C. for 1 h. After cooling the reaction mixture was poured on ice (1000 g) and the reaction mixture neutralized with potassium carbonate. The water phase was extracted with ether (5×200 ml). The organic phase was dried over MgSO4 and evaporated. The residue was purified by column chromatography (eluent: CH2Cl2 /CH3OH (9:1)), yielding 17 g of the title compound.

Provenance & Evidence