反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
To a solution of (14R,18R)-1-(diethoxyphosphoryl)-13-oxo-14-palmitamido-3,6,9-trioxa-16-thia-12-azanonadecane-18,19-diyl didodecanoate (1 eq) in DCM (0.1 M) was added trimethylsilyl bromide (10 eq). The reaction mixture was stirred at 25° C. overnight and concentrated. The crude mixture was purified by reverse phase high performance liquid chromatography (HPLC) with C4 column eluting with a gradient of 40-100% MeCN/10 mM NH4OAc (95:5) in 10 mM NH4OAc (pH 9) to give the title product as a white solid after lyophilizing. 1H NMR (CDCl3): δ 8.09 (br s, 2H), 5.18 (d, 2H), 4.62-4.70 (m, 2H), 4.36 (d, 2H), 4.13 (dd, 2H), 3.40-3.80 (m, 13H), 2.70-3.05 (m, 8H), 2.27-2.32 (m, 6H), 1.54-1.62 (m, 6H), 1.20-1.32 (m, 56H), 0.88 (t, 9H). LRMS [M+H]=1037.7.
WORKUP
后处理
- concentrationconcentrated
- customThe crude mixture was purified by reverse phase high performance liquid chromatography (HPLC) with C4 column
- washeluting with a gradient of 40-100% MeCN/10 mM NH4OAc (95:5) in 10 mM NH4OAc (pH 9)