c and then 20 ml of water was added the mixture was agitated for 15 minutes and 7 5 g of diisopropylethylamine was added the resulting mixture was agitated until all solids dissolved the reaction mixture was then cooled to u2212 5 to u2212 10 u00b0 c and 2 5 g of 3 7 aqueous formaldehyde was charged and the resulting mixture was agitated at u2212 5 to u2212 10 u00b0 c for 24 hours the reaction was monitored by hplc after the reaction was complete the reaction mixture was adjusted to ph 2 3 with 3m hydrochloric acid solution while maintaining the reaction temperature at u2212 10 to 5 u00b0 c with moderate agitation 125 ml of acetonitrile was added to the reaction mixture at 20 to 25 u00b0 c over 10 minutes the resulting mixture was stirred at 20 to 25 u00b0 c for 2 hours and then filtered the wet cake was washed with 20 ml of acetonitrile twice and dried for 18 hours in a vacuum oven at 20 to 25 u00b0 c to give 5 3 g of the title compound as a mixture of the di and trihydrochloride salt in u02dc 100 yield with a purity of ca 80 hplc area i e a compound of formula i where r 1 is u2014 ch 2 ch.