反应详情

To a solution of 4-methylaminomethylpiperidine-1-carboxylic acid tert-butyl ester (37 mg, 0.16 mmol) in anhydrous CH2Cl2 (3 mL) was added 2-pyridin-4-yl-pyrimidine-4-carbaldehyde (Preparation 2, 30 mg, 0.16 mmol) followed by NaBH(OAc)3 (38 mg, 0.18 mmol). The mixture was stirred vigorously at rt for 24 h, before being partitioned between CH2Cl2 (30 mL) and H2O (20 mL). The aqueous phase was extracted with CH2Cl2 (20 mL), then the combined organics were washed with brine (20 mL), dried (MgSO4), filtered and concentrated in vacuo. Flash column chromatography (EtOAc) gave the title compound. RT=2.36 min; m/z (ES+)=398 [M+H]+.

1. custombefore being partitioned between CH2Cl2 (30 mL) and H2O (20 mL)
2. extractionThe aqueous phase was extracted with CH2Cl2 (20 mL)
3. washthe combined organics were washed with brine (20 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo