反应详情

A solution of racemic 3-iodo-1-[1-(2-methoxyethyl)-3-piperidyl]-1H-pyrazolo[3,4-d]pyrimidin-4-amine (0.050 g, 0.00012 mol) in dimethoxyethane (2.5 mL) and water (5 mL) was treated with 4-phenoxyphenylboronic acid (0.029 g, 0.00014 mol), sodium carbonate (0.033 g, 0.00031 mol) and tetrakis(triphenylphosphine) palladium (0) (0.014 g, 0.00001 mol) at 80° C. for 20 hours. The organic solvent was removed in vacuo, and the crude material was purified by preparative RP-HPLC (Rainin C18, 8 μm, 300 A, 25 cm; 30% isocratic for five minutes, then 30%-60% acetonitrile-0.1M ammonium acetate over 15 min, 21 ml/min). The acetonitrile was removed in vacuo and the aqueous mixture was lyopholyzed to give 1-[1-(2-methoxyethyl)-3-piperidyl]-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine acetate as a white solid (0.038 g, 0.00007 mol).

1. customThe organic solvent was removed in vacuo
2. customthe crude material was purified by preparative RP-HPLC (Rainin C18, 8 μm, 300 A, 25 cm
3. wait30%-60% acetonitrile-0.1M ammonium acetate over 15 min
4. customThe acetonitrile was removed in vacuo