反应详情

The apparatus used in Example 1 was cleaned and charged with 95.1 g (0.50 mol) p-toluenesulfonic acid monohydrate and 750 mL toluene. The mixture was stirred to aid dissolution. MPP (88.13 g, 0.50 mol) was added slowly over 2 min. The reaction reached 38° C. The slurry was stirred for 1.5 hours, filtered, and the white solids allowed to air dry until partially dry (173.6 g). The solids were recrystallized from THF (approx. 1 L), filtered and dried. Dry weight=1782.1 g. Analysis by 1H NMR and FTIR verified the structure as that of the p-toluenesulfonic acid salt of MPP; mp=149°-150° C.; NaOH titration=108.83%; FW=348.48.g/mol; soluble in H2O, MeOH. DMSO and acetone. Calculated for C18H24N2O3S: C, 62.4%; H, 6.94%; N, 8.04%; S, 9.20%; O, 13.77%; Found: C, 62.075; H, 6.90%; N, 7.98%; S, 9.04%; O, 14.01%.

1. dissolutiondissolution
2. additionMPP (88.13 g, 0.50 mol) was added slowly over 2 min
3. customreached 38° C
4. stirringThe slurry was stirred for 1.5 hours
5. filtrationfiltered
6. customto air dry
7. customuntil partially dry (173.6 g)
8. customThe solids were recrystallized from THF (approx. 1 L)
9. filtrationfiltered
10. customdried
11. customDry weight=1782.1 g