反应详情

Z-Ile-Thr(tBu)-Thr(tBu)-Lys(Boc)-OPh (0.884 g, 1.0 mmol) was dissolved in 25 ml acetone and 4 ml H2O added followed by the addition of 3% H2O2 (1.16 ml, 1.0 mmol) and the solution stirred magnetically. The pH was adjusted to, and maintained at, 10.5 by the addition of 0.1N NaOH(a) after stirring at pH 10.5 for 1.5 h, 0.1N HCl was added until the reaction mixture reached pH 3. The white solid which formed was collected by filtration,(b) washed with H2O (~60 ml) and dried in vacuo to yield 0.781 g (96.6%); mp 174°-176° dec;(c)Rf 0.63 (ChCl3 :CH3OH:AcOH; 80-5-1); [α]D25 +13.66 (c 1, CH3OH). Anal: calc. for C41H69N5O11 (808.0): C, 60.94; H, 8.61; N, 8.67. Found: C, 60.83; H, 8.70; N, 8.93.

1. temperaturemaintained at, 10.5
2. stirringafter stirring at pH 10.5 for 1.5 h
3. customThe white solid which formed
4. filtrationwas collected by filtration,(b)
5. washwashed with H2O (~60 ml)
6. customdried in vacuo
7. customto yield 0.781 g (96.6%)