反应详情

To a solution of 480 mg of the amine III e1' in 5 ml of N,N-dimethylformamide is added 0.2 ml of methylisocyanate. The mixture is stirred at room temperature for 1 h, poured to water and extracted with ethyl acetate. The extracts are dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue is subjected to flash chromatography on silica gel in chloroform:methanol (9:1) and recrystallized from ethyl acetate to give 469 mg (88.0% yield) of the titled compound. mp. 87°-90° C.

1. extractionextracted with ethyl acetate
2. dry with materialThe extracts are dried over anhydrous sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customrecrystallized from ethyl acetate