反应详情

17.0 g H-D-Trp-Lys(BOC)-OMe are mixed with 80 ml THF. 9.2 g Z-Phg-OH are added to the grey suspension at RT. Addition of 4.4 g HOBt, rinsing with 20 ml THF. The turbid yellow solution is cooled down to 0° and a solution of 5.3 ml DICI in 15 ml THF added within 10 minutes. Stirring 2 hours at 0°, then 2 hours at RT. Then addition of a solution of 3.6 sulfuric acid in 57 ml water, extraction with 70 ml ethyl acetate, washing with water, saturated brine, 5% sodium hydrogencarbonate, 25% brine, drying over MgSO4 and evaporation. The white residue is stirred in 125 ml isopropyl acetate 2 hours at 40° and the suspension filtered. Drying of the residue at 40°: slightly yellow substance. HPLC: 96.3% b.a. (25.3 min).

1. washrinsing with 20 ml THF
2. temperatureThe turbid yellow solution is cooled down to 0°
3. additiona solution of 5.3 ml DICI in 15 ml THF added within 10 minutes
4. custom2 hours
5. customat RT
6. additionThen addition of a solution of 3.6 sulfuric acid in 57 ml water, extraction with 70 ml ethyl acetate
7. washwashing with water, saturated brine, 5% sodium hydrogencarbonate, 25% brine
8. dry with materialdrying over MgSO4 and evaporation
9. stirringThe white residue is stirred in 125 ml isopropyl acetate 2 hours at 40°
10. filtrationthe suspension filtered
11. customDrying of the residue at 40°
12. custom(25.3 min)