反应详情

温度

0 °C

2.5 g (13.1 mmol) of H-Phe(3-CN)—OH were dissolved in 100 ml of dioxane and, at 0° C., 13 ml (13 mmol) of 1N NaOH and 3.16 g (14.5 mmol) of Boc pyrocarbonate were added. The mixture was stirred at 0° C. for 20 min and then at room temperature for 4 h, during which a total of 7 ml (7 mmol) of 1N NaOH was added in portions, thus keeping the pH constant at 8-8.5. The solvent was removed in vacuo, and the residue was taken up in ethyl acetate, washed in each case 3× with 5% KHSO4 and 3× with NaCl-saturated water and then dried over Na2SO4. The solvent was removed in vacuo. A white solid was obtained as residue.

1. waitat room temperature for 4 h
2. customThe solvent was removed in vacuo
3. washwashed in each case 3× with 5% KHSO4 and 3× with NaCl-saturated water
4. dry with materialdried over Na2SO4
5. customThe solvent was removed in vacuo
6. customA white solid was obtained as residue