反应详情

温度

60 °C

N2-Butyl-8-(methyloxy)-3H-purine-2,6-diamine trifluoroacetate (192 mg, 0.547 mmol) and potassium carbonate (189 mg, 1.368 mmol) were suspended in DMF (3 ml) and heated to 60° C. for 1 hour. The reaction mixture was cooled to room temperature, 1-bromo-4-chlorobutane (0.063 ml, 0.547 mmol) added and the reaction stirred for a further 18 hours. Piperidine (0.054 ml, 0.547 mmol) and triethylamine (0.076 ml, 0.547 mmol) were added and the reaction mixture heated to 60° C. for 72 hours. The solvent was removed in vacuo and the residue partitioned between DCM (2 ml) and water (2 ml). The aqueous phase was re-extracted with DCM (2 ml) and the combined organic extracts were concentrated. The residue (ca. 200 mg) was dissolved in 1:1 MeOH:DMSO (1 ml) and purified by MDAP (Method A). The product containing fractions were evaporated in vacuo to give the impure title compound as a yellow gum (106 mg) which was used without further purification.

1. temperatureThe reaction mixture was cooled to room temperature
2. temperaturethe reaction mixture heated to 60° C. for 72 hours
3. customThe solvent was removed in vacuo
4. customthe residue partitioned between DCM (2 ml) and water (2 ml)
5. extractionThe aqueous phase was re-extracted with DCM (2 ml)
6. concentrationthe combined organic extracts were concentrated
7. dissolutionThe residue (ca. 200 mg) was dissolved in 1:1 MeOH
8. customDMSO (1 ml) and purified by MDAP (Method A)
9. additionThe product containing fractions
10. customwere evaporated in vacuo