反应详情

温度

0 °C

9.07 ml of N-ethylmorpholine and 16.05 g of DCC are added at 0° C. to a solution of 21.2 g of Z-D-Phe-OH, 9.6 g of HOBt and 17.9 g of HCl.H-Ser(tBu)-OtBu in 150 ml of dimethylformamide. The mixture is left to stir at 0° C. for one hour and to stand at room temperature overnight. The precipitate is filtered off with suction, and the filtrate is concentrated. The residue is partitioned between ethyl acetate and water. The ethyl acetate phase is extracted by shaking successively with saturated NaHCO3 solution, KHSO4 /K2SO4 solution and water, dried over Na2SO4 and concentrated. The substance crystallizes after trituration with petroleum ether.

1. waitThe mixture is left
2. waitto stand at room temperature overnight
3. filtrationThe precipitate is filtered off with suction
4. concentrationthe filtrate is concentrated
5. customThe residue is partitioned between ethyl acetate and water
6. extractionThe ethyl acetate phase is extracted
7. stirringby shaking successively with saturated NaHCO3 solution, KHSO4 /K2SO4 solution and water
8. dry with materialdried over Na2SO4
9. concentrationconcentrated
10. customThe substance crystallizes after trituration with petroleum ether