反应详情

Triethylamine (0.7 mL, 5 mmol) and 1-(1-chloro-2-hydroxy-3-propanyl)-4-(diphenylmethyl)piperazine (1.72 g, 5 mmol) was added to 4-mercapto-1H-pyrazolo[3,4-d]pyrimidine (0.78 g,5 mmol) in DMF (10 mL) in portions over a 5 min period. The solution was stirred under nitrogen for 4 days and DMF was removed under vacuum (50° C., 0.5 mmHg). The residue was dissolved in methylene chloride and the solution was washed with water (1+100 mL), saturated brine (1+100 mL) and the organic layer was filtered through celite and evaporated to give a foam (1.47 g). The crude material was eluted through silica gel using 10% methanol:methylene chloride which was extracted with methylene chloride and the organic layer was dried over Na2SO4 and evaporated and dried in vacuo to give the title compound, 0.36 g (13.9%), mp 87°-92° C. 400 MHz 1H NMR (CDCl3) δ:8.70 (s, 1H), 8.1 (s,1H), 7.4 (m, 5H), 7.15 (m,5H), 4.25 (s, 1H), 4.11 (m. 1H), 3.55 (m, 2H), 3.7-2.4 (m, 15H). DCI/MS (M+1) 5.17.

1. customDMF was removed under vacuum (50° C., 0.5 mmHg)
2. dissolutionThe residue was dissolved in methylene chloride
3. washthe solution was washed with water (1+100 mL), saturated brine (1+100 mL)
4. filtrationthe organic layer was filtered through celite
5. customevaporated