反应详情

0.9 g of carbonyldiimidazole was added to a solution of 1.8 g of 3-(3-hydroxymethyl-4-chloro-6-fluorophenyl)-1-amino-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione in 100 ml of tetrahydrofuran. After the reaction mixture had been stirred for 1 hour, 0.58 g of N-ethoxycarbonylhydroxylamine was added. The mixture was subsequently stirred for a further 14 hours at 20° C. whereupon the solvent was removed by distillation. The residue was taken up in 100 ml of methylene chloride. The resulting organic phase was washed with water, dried over sodium sulfate and finally concentrated. The crude product was purified by means of chromatography on silica gel (eluent: methylene chloride). Yield: 0.2 g.

1. stirringThe mixture was subsequently stirred for a further 14 hours at 20° C. whereupon the solvent
2. customwas removed by distillation
3. washThe resulting organic phase was washed with water
4. dry with materialdried over sodium sulfate
5. concentrationfinally concentrated
6. customThe crude product was purified by means of chromatography on silica gel (eluent: methylene chloride)