反应详情

7.34 g of diethyl cyanophosphonate were added to a mixture of 18.7 g of t-butyl N-[2-amino-5-(4-methoxymethoxy-2,3,5-trimethylphenoxy)phenyl]-N-methylcarbamate, 12.6 g of 4-(2,4-dioxothiazolidin-5-ylmethyl)phenoxyacetic acid, 4.55 g of triethylamine and 300 ml of anhydrous tetrahydrofuran. The resulting mixture was stirred at room temperature for 17 hours. The reaction mixture was concentrated by evaporation. Water was then added to the concentrate. After extraction with ethyl acetate, the extract was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by chromatography through a silica gel column (eluting solvent: n-hexane/ethyl acetate=1/1), whereby 23.1 g of the desired compound were obtained.

1. concentrationThe reaction mixture was concentrated by evaporation
2. additionWater was then added to the concentrate
3. extractionAfter extraction with ethyl acetate
4. dry with materialthe extract was dried over anhydrous sodium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customThe residue was purified by chromatography through a silica gel column (eluting solvent: n-hexane/ethyl acetate=1/1)