p-Toluenesulfonic acid monohydrate → HCID 86650660, compound

Participants

Reaction Steps

Add a solution of p-toluenesulfonic acid monohydrate (3.07 g, 16.1 mmol) in t-butylmethyl ether (25 mL) at 40° C. to a solution of 1-methyl-1-(6-trifluoromethyl-pyridin-2-yl)-ethylamine (3.20 g, 15.7 mmol) in t-butylmethyl ether (15 mL) at 35° C. Allow to cool to ambient temperature, and then add t-butylmethyl ether (10 mL). Stir at ambient temperature for approximately 1 hr. Filter and dry the resulting solid under vacuum at 40° C. to afford the title compound as an off white solid (5.17 g, 88%). 1H NMR (500 MHz, DMSO-d6) δ 8.42 (s, 3H), 8.22 (t, J=8.0 Hz, 1H), 7.98 (d, J=8.0 Hz, 1H), 7.93 (d, J=8.0 Hz, 1H), 7.46 (d, J=8.3 Hz, 2H), 7.10 (d, J=8.3 Hz, 2H), 2.27 (s, 3H), 1.63 (s, 6H).

Provenance & Evidence