反应详情

To a solution of (2-chloro-9-methyl-6-morpholin-4-yl-9H-purin-8-yl)acetaldehyde (117 mg, 0.40 mmol) in DCE (10 mL) was added 3-oxa-8-azabicyclo[3.2.1]octane (54 mg, 0.48 mmol) and powdered 4 Å molecular sieves. The reaction mixture was stirred at room temperature for 2 h, sodium triacetoxyborohydride (168 mg, 0.79 mmol) was added and the resulting mixture stirred for a further 16 h. The reaction mixture was filtered through Celite®, loaded onto an Isolute® SCX-2 cartridge, washed with MeOH then the desired product eluted with 2 M NH3 in MeOH. The resulting residue was purified by column chromatography (Si—PCC, 0-10% MeOH in DCM) to give the title compound as a pale yellow oil (80 mg, 51%). LCMS (Method H): RT=2.34 min, [M+H]+ 393.5

1. stirringthe resulting mixture stirred for a further 16 h
2. filtrationThe reaction mixture was filtered through Celite®
3. washwashed with MeOH
4. washthe desired product eluted with 2 M NH3 in MeOH
5. customThe resulting residue was purified by column chromatography (Si—PCC, 0-10% MeOH in DCM)