反应详情

温度

50 °C

2-(Butyloxy)-9-(5-chloropentyl)-8-(methyloxy)-9H-purin-6-amine (100 mg, 0.293 mmol), azetidine (0.020 ml, 0.293 mmol) and N,N-diisopropylethylamine (0.102 ml, 0.585 mmol) were dissolved in DMF (2 ml) and heated at 50° C. for 72 hours. The solvent was removed in vacuo and the residue partitioned between DCM (5 ml) and water (5 ml) and the layers separated using a hydrophobic frit. The aqueous phase was re-extracted with DCM (5 ml) and the combined organic extracts concentrated and the residue dissolved in 1:1 MeOH:DMSO (1 ml) and purified by MDAP (Method A). The product-containing fractions were evaporated under a stream of nitrogen to give the title compound as a clear gum (6.8 mg). LCMS (System B): tRET=1.26 min; MH+=363

1. customThe solvent was removed in vacuo
2. customthe residue partitioned between DCM (5 ml) and water (5 ml)
3. customthe layers separated
4. extractionThe aqueous phase was re-extracted with DCM (5 ml)
5. concentrationthe combined organic extracts concentrated
6. dissolutionthe residue dissolved in 1:1 MeOH
7. customDMSO (1 ml) and purified by MDAP (Method A)
8. customThe product-containing fractions were evaporated under a stream of nitrogen