Hydrochloric Acid → HCID 70548603, compound

Participants

Reaction Conditions

Reaction Steps

5 N Aqueous sodium hydroxide (20 cc) is added to a solution of (S)-3-[(5-methoxycarbonylmethyl-4-methylthiazol-2-yl)imino]-1,5,10,10a-tetrahydrothiazolo[3,4-b]isoquinoline (8.1 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, washed with water (5×25 cc), ethanol (3×15 cc) and diethyl ether (2×25 cc) and recrystallised by dissolving it in dimethylformamide (80 cc) at 150° C. and cooling to 0° C. The resulting crystals are filtered off, washed with dimethylformamide (10 cc), ethanol (4×15 cc) and diethyl ether (3×15 cc) and dried at 45° C. under reduced pressure (0.1 mm Hg; 0.013 kPa) to yield (S)-3-[(5-carboxymethyl-4-methylthiazol-2-yl)imino]-1,5,10,10a-tetrahydrothiazolo[3,4-b]-isoquinoline hydrochloride (4.8 g), as a white solid melting at about 250° C.

Provenance & Evidence