反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
Compound IV (2.0 g, 3.33 mmol) was dissolved in 0.4 M BF3.OEt2 in acetic acid (16.7 ml) and stirred at 25° C. for 4 hr. The solution was evaporated to a clear oil which was solidified by treatment with dry ether and drying over KOH. This material was dissolved in DMF (25 ml) and reacted with Et3N (0.47 ml) and Boc-Thr(Bzl)-Ser(Bzl)-OSu (1.89 g, 3.33 mmol) at 0° C for 1.5 hr and 25° C for 24 hr. The pH was adjusted to 8.0 (by wet pH paper) with Et3N when necessary during the course of reaction. The reaction was worked up as described above in Example 2 to yield a crystalline product from EtOAc and petroleum ether, yield 2.5 g (78.1%); mp 111°-115° C.; [α]D25 -4.8° (c 1, CHCl3). Anal. Calcd for C52H65N5O13 (968.12): C, 64.51; H, 6.76; N, 7.23. Found: C, 64.40; H, 6.60; N, 7.11.
WORKUP
后处理
- customThe solution was evaporated to a clear oil which
- dry with materialdrying over KOH
- dissolutionThis material was dissolved in DMF (25 ml)