反应详情

To a solution of 2-(2-ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purine (500 mg, 1.38 mmol) and TMEDA (312 μL, 2.07 mmol) in THF (10 mL) at −78° C. was added n-BuLi (660 μL, 1.65 mmol, 2.5M solution in hexanes) and the resulting mixture stirred for 30 min before the addition of a solution of 4-(methoxymethylcarbamoyl)piperidine-1-carboxylic acid tert-butyl ester (564 mg, 2.07 mmol) in THF (5 mL). The resulting mixture was stirred for 2 h then quenched with H2O and extracted with EtOAc. The combined organic phases were dried (MgSO4) and concentrated in vacuo. The resulting residue was triturated with EtOAc:cyclohexane and the mother liquors concentrated in vacuo affording the title compound as an oil (760 mg, 96%). LCMS (method A): RT 3.67 min [M+H]+ 557.3

1. customthen quenched with H2O
2. extractionextracted with EtOAc
3. dry with materialThe combined organic phases were dried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe resulting residue was triturated with EtOAc
6. concentrationcyclohexane and the mother liquors concentrated in vacuo