HRID1957306
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 5-fluorouridine (5-FU, 521 mg, 1.98 mmol) in 6 mL of anhydrous THF-DMF (1:1 under nitrogen was added N-(benzyioxycarbonyl)-L-valine (500 mg, 1.99 mmol), triphenylphosphine (521 mg, 1.98 mmol), and diisopropyl azodicarboxylate (402 mg, 1.98 mmol). The mixture was stirred overnight at 25 °C. The volatile components were removed under reduced pressure and the residue chromatographed over silica gel eluting with methyl alcohol:chloroform (1:5 ) to provide 5'-O-[N-(benzyloxycarbonyl)-L-valinyl]-5-fluorouridine (413 mg., 40% yield) as a white solid melting at about 64° C.-67° C.
WORKUP
后处理
- customThe volatile components were removed under reduced pressure
- customthe residue chromatographed over silica gel eluting with methyl alcohol:chloroform (1:5 )