反应详情

To a solution of 2-(2-ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-8-piperidin-4-yl-9H-purine hydrochloride (396 mg, 0.89 mmol) in THF (3 mL) and H2O (4 mL) was added 1M HCl to give pH 4 followed by NaCN (261 mg, 5.32 mmol) and propan-2-one (590 μL, 7.98 mmol). The resulting mixture was allowed to stir at r.t. for 16 h then partitioned between H2O and DCM. The organic phase was dried (phase separator) and concentrated in vacuo. The resulting residue was triturated with Et2O and the solid collected by filtration and dried in vacuo affording 2-{4-[2-(2-Ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purin-8-yl]piperidin-1-yl}-2-methylpropionitrile (316 mg, 69%). LCMS (method H): RT 2.64 min, [M+H]+ 514.4

1. customto give pH 4
2. customthen partitioned between H2O and DCM
3. customThe organic phase was dried (phase separator)
4. concentrationconcentrated in vacuo
5. customThe resulting residue was triturated with Et2O
6. filtrationthe solid collected by filtration
7. customdried in vacuo