反应详情

To a solution of N-isopropyl-2-[2-(4-methoxybenzylamino)-phenylamino]-N-(4-methoxy phenyl)-acetamide (3.25 g, 7.51 mmol) in THF (50 mL) cooled in an ice bath (<5° C.) was added 2-(phenyl-hydrazono) propandioyl dichloride (1.84 g, 7.51 mmol) in THF (50 mL) dropwise over 20 minutes. After complete addition, the solution was allowed to warm to room temperature and stirred overnight. The solvent was evaporated under reduced pressure and the resultant oil was dissolved in ethyl acetate (300 mL), washed with saturated sodium bicarbonate solution (100 mL) and brine (50 mL), dried over MgSO4, filtered and concentrated under reduced pressure to give the title compound (4.55 g, 7.51 mmol) as a yellow oil: 1H NMR (300 MHz, CDCl3): d 11.46 (s, 0.5H), 10.69 (s, 0.5H), 7.56-6.95 (m, 15H), 6.77-6.66 (m, 2H), 5.34 (m, 1H), 5.05 (m, 1H), 4.79 (m, 1H), 4.34-4.08 (m, 2H), 3.86 (s, 2H), 3.74 (s, 3H), 3.72 (s, 3H), 1.11 (m, 6H); TLC (EtOAc/Hexanes(2:3)): Rf =0.30.

1. additionAfter complete addition
2. customThe solvent was evaporated under reduced pressure
3. dissolutionthe resultant oil was dissolved in ethyl acetate (300 mL)
4. washwashed with saturated sodium bicarbonate solution (100 mL) and brine (50 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure