反应详情

Diisipropylazodicarboxylate (0.157 g) was added to a mixture of resin bound 3-[5-methyl-2-(1-naphthylmethyl)-4,6-dioxo-4,5,6,7-tetrahydro-2H-pyrazolo[3,4-d]pyrimidin-3-yl]benzoic acid (0.120 g), triphenylphosphine (0.204 g), and 2-chlorophenylmethanol in dry THF (2 mL) at −15° C. Reaction temperature was allowed to come to room temperature and shaken for 20 h. The resin was filtered, washed (3 times) DMF, CH2Cl2, MeOH, CH2Cl2, and dried in vacuum. The dry resin was treated with 15% TFA in dichloromethane (1 mL) for 2 h, and filtered and washed (2 times) with dichloromethane. Combined filtrates were concentrated, and dried in vacuum to give the title compound (0.062 g). Mass 548.80 (M+H).

1. additionDiisipropylazodicarboxylate (0.157 g) was added to a mixture of resin
2. customat −15° C
3. customReaction temperature
4. customto come to room temperature
5. filtrationThe resin was filtered
6. washwashed (3 times) DMF, CH2Cl2, MeOH, CH2Cl2
7. customdried in vacuum
8. additionThe dry resin was treated with 15% TFA in dichloromethane (1 mL) for 2 h
9. filtrationfiltered
10. washwashed (2 times) with dichloromethane
11. concentrationCombined filtrates were concentrated
12. customdried in vacuum