反应详情

2-(Butyloxy)-8-(methyloxy)-1H-purin-6-amine (300 mg, 1.264 mmol), (1-ethyl-4-piperidinyl)methanol (362 mg, 2.53 mmol) and tributylphosphine (0.624 ml, 2.53 mmol) were dissolved in THF (12 ml). 1,1′-(Azodicarbonyl)dipiperidine (638 mg, 2.53 mmol) was added and the reaction mixture stirred at rt overnight. The solvent was removed in vacuo and the residue purified by column chromatography, loading in dichloromethane and purified on Flashmaster II silica (Si) 20 g using a 0-100% ethyl acetate in cyclohexane+0-20% methanol (+1% Et3N) gradient over 30 mins. The appropriate fractions were combined and evaporated in vacuo. The material (300 mg) was dissolved in 1:1 MeOH:DMSO 3 ml and re-purified by Mass Directed AutoPrep (Method A). The solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus to give the title compound as a clear gum (60 mg). LCMS (System A): tRET=0.57 min; MH+ 363

1. customThe solvent was removed in vacuo
2. customthe residue purified by column chromatography, loading in dichloromethane
3. custompurified on Flashmaster II silica (Si) 20 g
4. customover 30 mins
5. customevaporated in vacuo
6. dissolutionThe material (300 mg) was dissolved in 1:1 MeOH
7. customDMSO 3 ml and re-purified by Mass Directed AutoPrep (Method A)
8. customThe solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus