反应详情

To a solution of (2-chloro-9-methyl-6-morpholin-4-yl-9H-purin-8-yl)acetaldehyde (167 mg, 0.57 mmol) in DCE (10 mL) was added 1-isopropylpiperazin-2-one (87 mg, 0.61 mmol) and powdered 4 Å molecular sieves. The reaction mixture was stirred at room temperature for 1 h, sodium triacetoxyborohydride (239 mg, 1.13 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% 2 M NH3/MeOH in DCM) to give the title compound as a pale yellow oil (51 mg, 33%). LCMS (Method H): RT=3.31 min, [M+H]+ 422.5

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% 2 M NH3/MeOH in DCM)