反应详情

温度

10 °C

A solution of N,N-diethyl-5,6-)methylenedioxy)phthalamic acid (3.00 g, 11.0 mmol) in tetrahydrofuran, under nitrogen at room temperature is treated with ethyl chloroformate (1.10 mL, 11.0 mmol), cooled to 10° C., treated with triethylamine (1.70 mL, 12.0 mmol), stirred for 30 minutes at 10° C., treated dropwise with a solution of α-methylvalinamide (1.43 g, 11.0 mmol) in tetrahydrofuran, stirred overnight at ambient temperatures, treated with water and concentrated in vacuo. The aqueous residue is extracted with ethyl acetate; the extracts are combined, washed with brine and saturated sodium bicarbonate, dried (MgSO4), and concentrated in vacuo to afford the title product as an amber foam 3.10 g (74.7%), identified by NMR and mass spectral analysis.

1. stirringstirred overnight at ambient temperatures
2. concentrationconcentrated in vacuo
3. extractionThe aqueous residue is extracted with ethyl acetate
4. washwashed with brine and saturated sodium bicarbonate
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo