反应详情

Gaseous HCl (0.22 g, 0.006 mole) is bubbled into 50 ml isopropanol. The resulting solution is added dropwise to ticlopidine free base (1.5 g, 0.005 mole) in 50 ml toluene, prepared, for example as described in Example A-3, maintaining the temperature below 40° C. during the addition. The reaction mixture is stirred for 1 hour, colled to about 5°-10° C. for 1 hour, and the precipitate separated by centrifugation. An acetone slurry is made of the precipitate, brought to reflux for 1 hour, and cooled to about 5°-10° C. for 1 hour. The precipitate, ticlopidine hydrochloride (Formula IV), is separated by centrifugation, dried at 65°-70° C. under vacuum, and recrystallized from methanol. (m.p. 206.5°-207.5° C.)

1. temperaturemaintaining the temperature below 40° C.
2. additionduring the addition
3. waitcolled to about 5°-10° C. for 1 hour
4. customthe precipitate separated by centrifugation
5. temperatureto reflux for 1 hour
6. temperaturecooled to about 5°-10° C. for 1 hour
7. customThe precipitate, ticlopidine hydrochloride (Formula IV), is separated by centrifugation
8. customdried at 65°-70° C. under vacuum
9. customrecrystallized from methanol