alcl3, aluminium chloride; trimethylaluminum; silica gel; hydrochlorid acid; toluene; dichloromethane; toluene; methanol; diethyl ether;
reactants are commercially availlable.
t illey, jefferson wright, us2009/264445, a1, (2009) example 112 (s)-2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid(3-methoxymethyl-[1,2,4]thiadiazol-5-yl)-amide to a stirred suspension of aluminum chloride (4.81 g, 0.090 mol) in toluene (33.5 ml) at 0°c. under argon was slowly added a solution of 2m trimethylaluminum in toluene (42 ml, 0.030 mol) maintaining a temperature below 10°c. the resulting mixture was allow ed to stir at room temperature for 2 h before a solution of 3-methoxyacetonitrile (5.56 g, 0.050 mol) in toluene (16.5 ml) was added. a fine light yellow precipitate formed and the resulting mixture w as warmed to 80°c. and allowed to stand for 20 h. the reaction mixture was cooled to room temperatu re and then slowly poured on to a cooled suspension of silica gel (40 g) in dichloromethane (100 ml) . the resulting mixture was stirred for 15 min, filtered and the silica gel pad washed well with methanol. the filtrate was evaporated and the residue was redissolved in a solution of dichloromethane/ methanol, filtered and evaporated which afforded a solid. the solid was suspended in a 3n hydrogen chloride solution in methanol (20 ml) and stirred vigorously while diethyl ether (500 ml) was added d ropwise. the resulting mixture was stirred at room temperature (30 min) decanted, washed with diethyl ether (250 ml) decanted and dried under vacuum which afforded 2-methoxy-acetamidine hydrochloride (4.66 g, 75percent) as a light yellow semisolid.
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