反应详情

To a solution of 31.5 g (15.5 mmol) 2-hydroxy-2-methyl-malonic acid monoethyl ester in 400 ml of tetrahydrofuran 16.9 g (17.1 mmol) of 2,2,2-trifluoroethylamine, 32.7 g (17.1 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride, 23.1 g (17.1 mmol) of 1-hydroxybenzotrizole hydrate and 58.1 ml (34.2 mmol) of N,N-diisopropyl-ethylamine were added. The mixture was stirred at room temperature for 18 h. The solvent was removed by distillation and the residue was extracted with water/ethylacetate. Chromatography on silicagel with heptane/ethylacetate 1:1 yielded 25.4 g (67%) 2-hydroxy-2-methyl-N-(2,2,2-trifluoroethyl)-malonamic acid ethyl ester, MS m/e (%): 242.1 (M−H, 100).

1. customThe solvent was removed by distillation
2. extractionthe residue was extracted with water/ethylacetate