反应详情

温度

0 °C

To a solution of Z-(D)-Nva-OH(380 mg), H-Leu-Arg(NO2)-Pro-Gly-NH2 (690 mg.) and HONB (300 mg.) in 5 ml. of dimethylformamide is added 340 mg. of DCC at 0°C with stirring. The mixture is stirred for 2 hours at 0°C and for additional 10 hours at room temperature. The reaction mixture is filtered to remove the formed dicyclohexyl-urea, and the filtrate is evaporated to dryness. The resulting residue is dissolved in 100 ml. of chloroform and the solution is washed with 4 % aqueous sodium bicarbonate solution and water. The washed solution is dried over anhydrous magnesium sulfate and evaporated to dryness. The residue is then triturated with a mixture of ethylacetate (25 ml.) and ether (25 ml.) to give a white powder, which is collected by filtration and reprecipitated from ethanol-ether: yield, 1.12 g., [α]D23 -50.5°(c=1.1 in Methanol), Rf1 =0.32.

1. filtrationThe reaction mixture is filtered
2. customto remove the formed dicyclohexyl-urea
3. customthe filtrate is evaporated to dryness
4. dissolutionThe resulting residue is dissolved in 100 ml
5. washof chloroform and the solution is washed with 4 % aqueous sodium bicarbonate solution and water
6. dry with materialThe washed solution is dried over anhydrous magnesium sulfate
7. customevaporated to dryness
8. customThe residue is then triturated with a mixture of ethylacetate (25 ml.) and ether (25 ml.)
9. customto give a white powder, which
10. filtrationis collected by filtration
11. customreprecipitated from ethanol-ether
12. customyield