反应详情

温度

22.5 °C

A reactor was charged with 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene free base (2 g; 0.0095 mole, 1.0 equiv.) and methanol (60 mL, 30 mL/g). The mixture was stirred at 20 to 25° C. until completely dissolved. A second reactor containing a solution of L-tartaric acid (1.55 g, 0.0103 mole, 1.1 equiv.) dissolved in methanol (60 mL, 30 mL/g) was heated to reflux in methanol (i.e., 60 to 66° C.). The free base solution was added to the L-tartaric acid solution at methanolic reflux temperature over 20 minutes. The resulting slurry was cooled to 20 to 25° C. over a 1 hour period. The reaction mixture was allowed to stir for approximately 2 hours followed by isolation of the product by filtration. The solid product was washed with methanol (10 mL), then dried under vacuum at 30 to 35° C. to give 3.3 grams (97%) of 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene L-tartrate Form A. The identity as Form A was determined by PXRD as compared with standard samples.

1. dissolutionuntil completely dissolved
2. temperaturewas heated
3. temperatureThe resulting slurry was cooled to 20 to 25° C. over a 1 hour period
4. stirringto stir for approximately 2 hours
5. filtrationfollowed by isolation of the product by filtration
6. washThe solid product was washed with methanol (10 mL)
7. customdried under vacuum at 30 to 35° C.