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) was added and the reaction stirred for a further 18 hours. Hexahydro-1H-azepine (54.2 mg, 0.547 mmol) and triethylamine (0.076 ml, 0.547 mmol) were added and the reaction mixture heated to 60° C. for 18 hours. The solvent was removed in vacuo and the residue was partitioned between DCM (5 ml) and water (5 ml). The aqueous phase was re-extracted with DCM (5 ml) and the combined organic extracts were concentrated in vacuo. The residue was dissolved in 1:1 MeOH:DMSO (2 ml) and purified in 2 injections by MDAP (Method B). This provided material (74 mg) that was still impure and which was repurified by MDAP (Method A). The product containing fractions were evaporated under a stream of nitrogen to give the title compound as a clear gum (13 mg).

1. temperatureThe reaction mixture was cooled to room temperature
2. temperaturethe reaction mixture heated to 60° C. for 18 hours
3. customThe solvent was removed in vacuo
4. customthe residue was partitioned between DCM (5 ml) and water (5 ml)
5. extractionThe aqueous phase was re-extracted with DCM (5 ml)
6. concentrationthe combined organic extracts were concentrated in vacuo
7. dissolutionThe residue was dissolved in 1:1 MeOH
8. customDMSO (2 ml) and purified in 2 injections by MDAP (Method B)
9. customwhich was repurified by MDAP (Method A)
10. additionThe product containing fractions
11. customwere evaporated under a stream of nitrogen