反应详情

To a suspension of 4-(3-hydroxy-pyridin-2-yl)-cyclohexanone (as prepared in step C, 1 eq.) and N-(azetidin-3-yl)-2-((6-(trifluoromethyl)quinazolin-4-yl)amino)acetamide (as prepared in the previous step, tris TFA salt, 1 eq.) in DCM was added TEA (3 eq.). After stirring at room temperature 30 minutes, NaBH(OAc)3 (3 eq) was added and the mixture was stirred overnight. The reaction was quenched with saturated sodium bicarbonate solution and partially concentrated. Extraction with ethyl acetate followed by concentration of the organic layer in vacuo yielded a residue which was purified by flash chromatography (silica gel, 0-20% 7 N NH3-MeOH/Ethyl acetate) to afford the product as a solid, mixture of isomers.

1. customas prepared in the previous step
2. stirringthe mixture was stirred overnight
3. customThe reaction was quenched with saturated sodium bicarbonate solution
4. concentrationpartially concentrated
5. extractionExtraction with ethyl acetate
6. customyielded a residue which
7. customwas purified by flash chromatography (silica gel, 0-20% 7 N NH3-MeOH/Ethyl acetate)
8. customto afford