Hydrochloric Acid → HCID 70548735, compound

Participants

Reaction Conditions

Reaction Steps

5 N Aqueous sodium hydroxide (20 cc) is added to a solution of (S)-3-[(5-ethoxycarbonylmethylthiazol-2-yl)imino]-1,5,10,10a-tetrahydrothiazolo[3,4-b]-isoquinoline (7.9 g) in ethanol (60 cc). The mixture is heated under reflux for two hours. After cooling to 20° C., it is acidified by adding 12 N hydrochloric acid (d=1.19; 10 cc). The resulting precipitate is filtered off and washed with water (3×50 cc) and then with ethanol (50 cc) and diethyl ether (20 cc). The product is recrystallised by dissolving it in dimethylformamide (15 cc) at 70° C., adding ethanol (80 cc) and cooling to 0° C. The resulting crystals are filtered off, washed with ethanol (50 cc) and then with diethyl ether (20 cc) and dried at 50° C. under reduced pressure (0.1 mm Hg; 0.013 kPa) to yield (S)-3-[(5-carboxymethylthiazol-2-yl)imino]-1,5,10,10a-tetrahydrothiazolo[3,4-b]isoquinoline hydrochloride (6.8 g), melting at about 240° C.

Provenance & Evidence