反应详情

温度

50 °C

3-Bromopentane (0.1 mmol) was weighed into a tube and an aliquot (0.4 ml, 0.12 mmol) of a solution of 2-(butyloxy)-8-(methyloxy)-9-[4-(4-piperidinyl)butyl]-9H-purin-6-amine (0.452 g mg, 1.2 mmol) suspended in DMF (4.8 ml) was added. DIPEA (40 μl, 0.229 mmol) was added and heated at 50° C. for 18 hours. An additional portion of 3-bromopentane (15 μl) and DIPEA (40 μl) was added and heating continued for a further 18 hours. Potassium carbonate (46 mg) was added and heating continued for a further 72 hours. DMSO (200 uL) was added and the resultant mixture filtered, the solution was purified by Mass Directed AutoPrep (Method A). The solvent was evaporated in vacuo using the Genevac. The residue was redissolved in 4M HCl/dioxane (0.2 ml), capped and stood at room temperature for 18 hours. The solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus. The sample was dissolved in 1:1 DMSO:MeOH and purified by MDAP (Method C) and the solvent was evaporated in vacuo using the Genevac. The material was redissolved in methanol (0.5 ml), and applied to a 0.1 g aminopropyl SPE (preconditioned with methanol, 1.5 ml). The cartridge was eluted with methanol (1.5 ml), the solvent was removed to give the title compound (5.9 mg).

1. additionwas added
2. temperatureheating
3. temperatureheating
4. waitcontinued for a further 72 hours
5. filtrationthe resultant mixture filtered
6. customthe solution was purified by Mass Directed AutoPrep (Method A)
7. customThe solvent was evaporated in vacuo
8. dissolutionThe residue was redissolved in 4M HCl/dioxane (0.2 ml)
9. customcapped
10. waitstood at room temperature for 18 hours
11. customThe solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus
12. dissolutionThe sample was dissolved in 1:1 DMSO
13. customMeOH and purified by MDAP (Method C)
14. customthe solvent was evaporated in vacuo
15. dissolutionThe material was redissolved in methanol (0.5 ml)
16. washThe cartridge was eluted with methanol (1.5 ml)
17. customthe solvent was removed