反应详情

In 10 ml of trifluoroacetic acid is dissolved 0.80 g of BOC-Gly-MePhe-NHNHCSNH2, and the solution is shaken for 10 minutes, concentrated, treated with ether and filtered to obtain a powder. This powder is dissolved in 10 ml of DMF, and after ice-cooling, the solution is neutralized with 10 ml of DMF and 0.05 g BOC-(D)-Gln-OH, 0.40 g of HONB and 0.45 g of DCC are added. The mixture is stirred for 20 hours. The precipitated DCU is filtered off, the solvent distilled off and the residue dissolved in n-butanol. The solution is washed with a saturated aqueous solution of sodium hydrogen carbonate and water in that order and dried over anhydrous sodium sulfate. The solvent is distilled off and the residue is treated with ether and filtered to obtain a powder. Yield 0.73 g; m.p. 120°-123° C.; [α]D24 -46.0° (c=1.0, DMF); Rf1 0.18.

1. concentrationconcentrated
2. additiontreated with ether
3. filtrationfiltered
4. customto obtain a powder
5. temperatureafter ice-cooling
6. additionare added
7. stirringThe mixture is stirred for 20 hours
8. filtrationThe precipitated DCU is filtered off
9. distillationthe solvent distilled off
10. dissolutionthe residue dissolved in n-butanol
11. washThe solution is washed with a saturated aqueous solution of sodium hydrogen carbonate and water in that order
12. dry with materialdried over anhydrous sodium sulfate
13. distillationThe solvent is distilled off
14. additionthe residue is treated with ether
15. filtrationfiltered
16. customto obtain a powder