反应详情

A solution of 2,2-dimethyl-4-(6-morpholino-5-nitropyridin-3-yl)morpholine (490 mg, 1.52 mmol; described herein) in 30 mL MeOH was reduced in a Thalles H-Cube® hydrogenator using a 10% Pd/C CatCart column (20 bar, 25° C., 1 mL/min flow rate.) The reaction mixture was then concentrated, diluted with EtOAc, and extracted with 1M HCl. The aq. layer was washed with DCM and basified with 1M NaOH. The product was extracted with EtOAc, dried (magnesium sulfate), and concentrated, affording 5-(2,2-dimethylmorpholino)-2-morpholinopyridin-3-amine as a beige powder. Mass Spectrum (ESI) m/e=293.2 (M+1).

1. concentrationwas then concentrated
2. additiondiluted with EtOAc
3. extractionextracted with 1M HCl
4. washThe aq. layer was washed with DCM and basified with 1M NaOH
5. extractionThe product was extracted with EtOAc
6. dry with materialdried (magnesium sulfate)
7. concentrationconcentrated