Methylamine → HCID 23582858, compound

Participants

Reaction Conditions

Reaction Steps

The title compound was prepared from product from step 1 (0.6 g, 1.9 mmol) and methyl amine (40% in water, 16.2 mL, 0.47 mol) in acetonitrile (6 mL) was heated to 60° C. for 7 h, and then room temperature for 16 h. The mixture was extracted with ethyl acetate. The combined organic portions were acidified with 10% HCl to pH to 1, and stirred at 0° C. for 1 h. The product was collected on a filter, washed with 1N HCl, water and hexane. After drying under vacuum, the title compound (0.5 g, 79%)as a hydrochloride salt. 1H NMR (400 MHz, CD3OD) δ 7.66-7.60 (m, d, J=9.2 Hz, 4H), 7.43-7.39 (m, 1H), 7.23-7.18 (m, d, J=9.2 Hz, 3H), 4.24 (t, J=6 Hz, 2H), 3.27 (t, J=6 Hz, 2H), 2.77 (s, 3H), 2.24 (m, 2H); MS (APCI) m/z 316 (M+1, 100); LC/MS (APCI) m/z: 99%.

Provenance & Evidence