反应详情

A solution of 3-iodo-1H-pyrazolo[3,4-d]pyrimidin-4-amine (400 mg, 1.53 mmol) and K2CO3 (1 g, 6 mmol) in DMF (5 ml) was stirred at room temperature under an argon atomosphere. Iodocyclopentane (1.0 g, 0.0084 mol) was added with a syringe. Reaction was refluxed under argon atmosphere for 2 hours. Solid K2CO3 was removed by filtration. Solvent was partially removed in vacuo. Sodium citrate (50 ml) was added and reaction was extracted with EtOAc. Organic phases concentrated in vacuo and purified using silica gel column chromatography [MeOH—CH2Cl2, 5:95] yielding BA80 (300 mg, 60% yield). ESI-MS (M+H)+ m/z calcd 330.0, found 330.0.

1. customReaction
2. temperaturewas refluxed under argon atmosphere for 2 hours
3. customSolid K2CO3 was removed by filtration
4. customSolvent was partially removed in vacuo
5. additionSodium citrate (50 ml) was added
6. customreaction
7. extractionwas extracted with EtOAc
8. concentrationOrganic phases concentrated in vacuo
9. custompurified
10. customyielding BA80 (300 mg, 60% yield)