反应详情

According to process “A′”, 0.12 g of the trifluoroacetic acid salt of compound 267.4 was dissolved at room temperature in 5 ml of dry tetrahydrofuran, admixed with 0.17 ml of triethylamine and then admixed dropwise with a solution of 0.10 g of methyl isocyanatomethylpropionate in 2 ml of dry tetrahydrofuran. The mixture was stirred at room temperature for 2 hours. For workup, the mixture was concentrated under reduced pressure, and the residue was stirred with water, filtered, washed with water and dried. Methyl 2-[3-(4-fluoro-3-thiophen-2-ylphenyl)ureido]-2-methylpropionate (267.3) was obtained. Molecular weight 336.39 (C16H17FN2O3S); retention time Rt=1.46 min. [F]; MS (ESI): 337.05 (MH+).

1. concentrationFor workup, the mixture was concentrated under reduced pressure
2. stirringthe residue was stirred with water
3. filtrationfiltered
4. washwashed with water
5. customdried