反应详情

23 g (0.086 mol) of prolyl-arginine (2) are dissolved in 100 ml of water and to this solution under stirring there is added a solution of 53 g (0.1 mol) of pentafluorophenyl ester of tert.butyloxycarbonyl-Nε -benzyloxycarbonyl-lysine in 300 ml of dioxane. 2 hours thereafter the solvent is evaporated and the residue is dissolved in 150 ml of dimethylformamide and stirred at room temperature (20° C.) for 48 hours. Then dimethylformamide is evaporated to 1/3 of its volume and the solution is poured into one liter of ether. After 2 hours the resulting residue is filtered-off, washed on the filter with ether and dried in vacuum. After reprecipitation from a mixture ethylacetate-ethanol-ether (3:1:30) there are obtained 47 g (74%) of the product (3) having the following properties: M.p. 90° C., [α]D20 -39.0° (c 1.0; 10% CH3COOH); Rf =0.51 (A, "Eastman"), 0.82 (B, "Eastman"); EHis =0.34 (pH=2.4).

1. custom2 hours thereafter the solvent is evaporated
2. dissolutionthe residue is dissolved in 150 ml of dimethylformamide
3. stirringstirred at room temperature (20° C.) for 48 hours
4. customThen dimethylformamide is evaporated to 1/3 of its volume
5. additionthe solution is poured into one liter of ether
6. washwashed on the
7. filtrationfilter with ether
8. customdried in vacuum
9. customAfter reprecipitation from a mixture ethylacetate-ethanol-ether (3:1:30) there