Cesium carbonate → HCID 9909865, compound

Participants

Reaction Conditions

Reaction Steps

To the product of Example 4 Step a) (2.67 g) and (2-methyl-2H-1,2,4-triazol-3-yl)methanol (prepared as described in EP-A-421210) (0.93 g) in dry dimethylsulfoxide (10 ml) was added caesium carbonate (3.14 g), and the mixture stirred at 50° C. under an atmosphere of dry nitrogen for 24 hours. On cooling to room temperature, the mixture was partitioned between ethyl acetate and water. The organic phase was separated, washed with water, evaporated at reduced pressure, and the residue chromatographed on silica gel (eluent 2.5% methanol-dichloromethane). The product was crystallised from ethyl acetate/diethyl ether/isohexane, to afford the title compound as a colourless solid. 1H NMR (500 MHz, DMSO-6) δ1.39 (9H, s), 3.74 (3H, s), 5.50 (2H, s), 7.46 (1H, m), 7.88 (1H, m), 7.90 (1H, s), 8.17 (1H, s); MS (ES+) m/z 418 [MH]+.

Provenance & Evidence