反应详情

To a solution of N2-(2,4-dimethyl-6-nitrophenyl)-N1,N1-dimethylglycinamide from Step A (2.54 g, 10.1 mmol) in EtOH (50 mL) was added 10% Pd/C (500 mg). The reaction mixture was stirred under a hydrogen atmosphere (ca. 1 atm) for 72 h, then filtered through a Celite pad, washing with EtOH, and the filtrate was concentrated under reduced pressure. The crude product was purified by silica gel chromatography, eluting with a gradient of hexane:EtOAc —100:0 to 0:100, to give the title compound. MS: m/z=222 (M+1).

1. filtrationfiltered through a Celite pad
2. washwashing with EtOH
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe crude product was purified by silica gel chromatography
5. washeluting with a gradient of hexane:EtOAc —100:0 to 0:100