反应详情

温度

50 °C

2-(Butyloxy)-9-(4-chlorobutyl)-8-(methyloxy)-9H-purin-6-amine (100 mg, 0.305 mmol), azetidine (0.021 ml, 0.305 mmol) and N,N-diisopropylethylamine (0.107 ml, 0.610 mmol) were dissolved in DMF (2 ml) and heated at 50° C. for 48 hours. LCMS indicated the reaction to be incomplete and additional azetidine (0.021 ml, 0.305 mmol) and N,N-diisopropylethylamine (0.107 ml, 0.610 mmol) were added and the reaction mixture heated at 50° C. for a further 48 hours. The mixture was then partitioned between DCM (4 ml) and water (4 ml) and the layers separated using a hydrophobic frit. The aqueous phase was re-extracted with DCM (4 ml) and the combined organic extracts were concentrated and the residue 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 (7.6 mg).

1. customthe reaction
2. temperaturethe reaction mixture heated at 50° C. for a further 48 hours
3. customThe mixture was then partitioned between DCM (4 ml) and water (4 ml)
4. customthe layers separated
5. extractionThe aqueous phase was re-extracted with DCM (4 ml)
6. concentrationthe combined organic extracts were concentrated
7. customthe residue purified by MDAP (Method A)
8. customThe product-containing fractions were evaporated under a stream of nitrogen