反应详情

温度

0 °C

In 150 ml of chloroform were dissolved 26.5 g of Boc-Phe-OH and 22.9 g of H-Phe-OEt.HCl, to which 18.4 ml of WSC was added under cooling at 0° C. This was then subjected to stirring for 2 hours at -10° C., then 15 hours at room temperature. The reaction solution was concentrated in vacuo and the residue was dissolved in 20 ml of ethyl acetate, washed successively with 1 N HCl, water, 5% aqueous NaHCO3 solution and water, dried over Na2SO4 then again concentrated in vacuo. The thus obtained residue was added to n-hexane and the resultant amorphous precipitate was collected, and was recrystallized from n-hexane, which gave 37 g (yield=84%) of the title product. m.p. 106.5°-107.5° C. [α]D25 -9.7° (C 1.3, DMF). Analysis--Calculated for C25H32O5N2 : C, 68.16; H, 7.32; N, 6.36. Found: C, 67.85; H, 7.32; N, 6.49.

1. custom15 hours
2. customat room temperature
3. concentrationThe reaction solution was concentrated in vacuo
4. dissolutionthe residue was dissolved in 20 ml of ethyl acetate
5. washwashed successively with 1 N HCl, water, 5% aqueous NaHCO3 solution and water
6. dry with materialdried over Na2SO4
7. concentrationthen again concentrated in vacuo
8. additionThe thus obtained residue was added to n-hexane
9. customthe resultant amorphous precipitate was collected
10. customwas recrystallized from n-hexane, which