反应详情

and H2N-Cys(Trt)-OMe 26. 7.2 g (12.3 mmol) of Fmoc-Cys(Trt)-OH was dissolved in 70 ml of MeOH and added 1.5 ml of conc. sulfuric acid. The reaction mixture was refluxed for 4 hr, the solvent was removed. The mixture was then mixed with ethyl acetate, and washed with water, saturated NaHCO3, and brine. Removing the solvent under vacuum gave 25 as a white foamy solid. The crude product was dissolved in 20 ml of 20% piperidine solution in DMF. After 2 hr, the solvent was removed. Silicagel chromatography (CH2Cl2: MeOH=10:1) gave 4.0 g (86% two step yield) of 26 as a white solid.

1. temperatureThe reaction mixture was refluxed for 4 hr
2. customthe solvent was removed
3. additionThe mixture was then mixed with ethyl acetate
4. washwashed with water, saturated NaHCO3, and brine
5. customRemoving the solvent under vacuum