Triethylamine → HCID 131716237, compound

Participants

Reaction Steps

To a solution of 1.2 g of 3-aminoquinuclidine and 1.2 g triethylamine in 50 ml of chloroform is added a solution of 3.45 g of 6-chloro-3,4-dihydro-2-methyl-3-oxo-4-(2phenylethyl) -2H-1,4-benzoxazine-8-carboxylic acid chloride in 20 ml of chloroform under cooling and stirring followed by stirring at room temperature for 4 hours. The resultant solution is washed with water, aqueous sodium hydrogen carbonate and then water, and dried over magnesium sulfate. After the solvent is distilled off under reduced pressure, the residue is recrystallized from ethanolisopropyl ether and treated with ethanolic hydrochloric acid to give 6-chloro-3,4-dihydro-2-methyl-3-oxo-4-(2-phenylethyl)-N-(3-quinuclidinyl)-2H-1,4-benzoxazine-8-carboxamide hydrochloride hemihydrate, melting at 207° C. with decomposition.

Provenance & Evidence