反应详情

A solution of 0.517 g of 2(R)-[1(S)-(tert-butoxycarbonyl)-4-phenylbutyl]-4-methylvalerohydrazide in 5 ml of dichloromethane was treated with 0.302 g of methyl (S)-(+)-2-isocyanato-3-methylbutyrate and 0.3 ml of N-ethylmorpholine. The mixture was stirred at room temperature for 4 hours and then the solution was washed with 5% aqueous citric acid solution, saturated sodium chloride solution, dried over anhydrous magnesium sulphate and evaporated. The residue was dissolved in 5 ml of toluene containing 0.2 ml of triethylamine. The mixture was heated at reflux for 24 hours. The solution was cooled, diluted with ethyl acetate and washed with 5% aqueous citric acid solution, saturated sodium chloride solution, dried over anhydrous magnesium sulphate, and evaporated. The residue was triturated with ether and there was obtained 0.468 g of 2(R)-[1(S)-(tert-butoxycarbonyl)-4-phenylbutyl]-N-(4(S)-isopropyl-2,5-dioxo-1-imidazolidinyl)-4-methylvaleramide in the form of a white solid.

1. washthe solution was washed with 5% aqueous citric acid solution, saturated sodium chloride solution
2. dry with materialdried over anhydrous magnesium sulphate
3. customevaporated
4. dissolutionThe residue was dissolved in 5 ml of toluene containing 0.2 ml of triethylamine
5. temperatureThe mixture was heated
6. temperatureat reflux for 24 hours
7. temperatureThe solution was cooled
8. additiondiluted with ethyl acetate
9. washwashed with 5% aqueous citric acid solution, saturated sodium chloride solution
10. dry with materialdried over anhydrous magnesium sulphate
11. customevaporated
12. customThe residue was triturated with ether