反应详情

A mixture of 2-chloro-4-morpholin-4-ylthieno[3,2-d]pyrimidine-6-carbaldehyde (400 mg, 1.42 mmol), 3,3-dimethyl-1-oxetan-3-ylpiperazine (290 mg, 1.71 mmol) and 4 Å powdered molecular sieves (500 mg) in DCE (20 mL) were allowed to stir at r.t. 3 h before the addition of sodium triacetoxyborohydride (420 mg, 1.98 mmol). The resulting mixture was allowed to stir for 18 h then filtered through Celite®. The filtrate was loaded onto an Isolute® SCX-2 cartridge which was washed with MeOH and the product eluted with 2M NH3/MeOH. The resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%) affording the title compound as a cream solid (305 mg, 49%)._LCMS (method H): RT 2.12 min, [M+H]+ 438.3

1. stirringto stir for 18 h
2. filtrationthen filtered through Celite®
3. washwas washed with MeOH
4. washthe product eluted with 2M NH3/MeOH
5. customThe resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%)