反应详情

温度

-78 °C

2-(biphenyl-4-ylmethyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (203 mg, 0.523 mmol) is dissolved in anhydrous THF (5 mL), and then cooled to −78° C. 1.8 M solution of LDA in THF (600 uL) is added dropwise with rigorous stirring at −78° C., followed by the addition of iodine (160 mg, 0.63 mmol) in THF. The reaction mixture is stirred at −78° C. for an hour, and then is allowed to warm up to room temperature before quenching. The mixture is poured into saturated NH4Cl solution, and then extracted with ethyl acetate three times. The combined organic phase is washed with potassium iodide aqueous solution (1 M), water, and then dried over Na2SO4. Solvent is removed under reduced vacuum to give crude product was white solids. MS (ESI) m/z 515.1 [M+H]+.

1. stirringThe reaction mixture is stirred at −78° C. for an hour
2. temperatureto warm up to room temperature
3. custombefore quenching
4. additionThe mixture is poured into saturated NH4Cl solution
5. extractionextracted with ethyl acetate three times
6. washThe combined organic phase is washed with potassium iodide aqueous solution (1 M), water
7. dry with materialdried over Na2SO4
8. customSolvent is removed under reduced vacuum
9. customto give crude product