反应详情

温度

-15 °C

Dibenzylphosphory-L-alanyl-L-proline (1.4 g, 3.2 m mole), HOBt (476 mg, 3.5 m mole) and D-alanine benzylester p-toluene sulfonic acid salt (1.3 g, 3.5 m mole) were dissolved in DMF (5 ml), and WSC (0.64 ml) was added thereto while cooling to -15° C. The reaction was carried out for 3 hours under cooling and then overnight at room temperature. To the reaction solution ethyl acetate (100 ml) was added and the mixture was washed with 1N hydrochloric acid, 5% sodium bicarbonate and water in order. The mixture was dried with anhydrous sodium sulfate and the thus obtained solution was distilled under reduced pressure to give an oily dibenzylphosphoryl-L-alanyl-L-prolyl-D-alanine benzylester material.

1. temperatureunder cooling
2. customovernight
3. customat room temperature
4. washthe mixture was washed with 1N hydrochloric acid, 5% sodium bicarbonate and water in order
5. dry with materialThe mixture was dried with anhydrous sodium sulfate
6. distillationthe thus obtained solution was distilled under reduced pressure