反应详情

To a mixture of Boc-D-Trp(CH3)-OH (1.59 g), HCl.H-D-Phe-OCH3 (1.08 g) and HOBT (0.81 g) in DMF (20 ml) was added WSCD (0.93 g) under ice-bath cooling. After being stirred for 2 hours at room temperature, the mixture was concentrated in vacuo and the residue was dissolved in ethyl acetate (50 ml). The solution was washed with 0.5N hydrochloric acid (20 ml), water (20 ml), saturated sodium bicarbonate (20 ml) and water (20 ml×2) successively, dried over magnesium sulfate and evaporated in vacuo. The residue was triturated with ether to give Boc-D-Trp(CH3)-D-Phe-OCH3 (1.45 g).

1. temperaturecooling
2. concentrationthe mixture was concentrated in vacuo
3. dissolutionthe residue was dissolved in ethyl acetate (50 ml)
4. washThe solution was washed with 0.5N hydrochloric acid (20 ml), water (20 ml), saturated sodium bicarbonate (20 ml) and water (20 ml×2) successively
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue was triturated with ether