Benzyl Alcohol → Benzyl Alcohol

Participants

Reaction Conditions

Reaction Steps

1-[4-(5-Cyanoindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine (4 g) in benzyl alcohol (36 ml) was heated to 35-40° C. under inert gas atmosphere. The clear solution was filtered through microfiber paper and washed with benzyl alcohol (4 ml). The filtrate was stirred at 20-25° C. for about 30 minutes. To the thin suspension was charged conc. HCl (0.91 g, 0.98 eq.) and a clear solution was obtained. Following stirring for about 10 minutes a thick suspension formed, which was allowed to stir at 20-25° C. for 17 hours. The suspension was heated to about 95° C. and stirred for about 6.5 hours whereupon the suspension became thin. The resulting suspension was cooled to 30-35° C. and stirred for about 1 hour. The solid was filtered, washed with benzyl alcohol (8 ml) and MTBE (3×8 ml) and dried in vacuo at 35-40° C. for about 3 hours to afford 4.5 g mono solvate of 1-[4-(5-cyanoindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine hydrochloride with benzyl alcohol.

Provenance & Evidence