Phosphorus oxychloride → HCID 10631964, compound

Participants

Reaction Conditions

Reaction Steps

Phosphorus oxychloride (6.7 ml, 39.1 mmoles) was added to a solution of compound 5b (3.00 g, 16.3 mmoles) and benzyltriethylammonium chloride (14.90 g, 65.2 mmoles) in acetonitrile (60 ml). The mixture obtained was agitated at 40° C. for 30 minutes and heated under reflux for 1 hour. After evaporation of the solvent, 60 ml of water was added and the mixture agitated at ambient temperature for 3 hours. The yellow precipitate was collected, washed with cyclohexane (3×6 ml) and dried to give compound 6b (2.4 g, 74%) in the form of pale yellow crystals: NMR-1H (DMSO-d6) δ 13.19 (1H, s, NH-1), 7.73 (1H, s, H-6), 2.56 (2H, q, L=7.5 Hz, CH2CH3), 1.16 (3H, t, J=7.5 Hz, CH2CH3 ).

Provenance & Evidence