HRID19467
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
- 110 °C
PROCEDURE
实验过程
3-(β-D-Ribofuranosyl)-pyridin-2(1H)-one (342 mg, 1.5 mmol) (Matulic-Adamic, J., Beigelman, L., Tetrahedron Lett., 1997, 38, p. 203-206; Ishikawa, M., Hirao, I., Yokoyama, S., Tetrahedron Lett., 2000, 41, p. 3931-3934), iodine (573 mg, 2.3 mmol) and potassium iodide (KI) (657 mg, 7.9 mmol) were added to 50 mM sodium carbonate (36 ml) and heated at 110° C. for 12 hours. After the reaction, dichloromethane was added to separate the aqueous layer, followed by washing with dichloromethane. The aqueous layer was concentrated under reduced pressure and then purified by C18 reversed-phase HPLC to give 3-(β-D-ribofuranosyl)-5-iodopyridin-2(1H)-one (155 mg).
WORKUP
后处理
- additionwas added
- customto separate the aqueous layer
- washby washing with dichloromethane
- concentrationThe aqueous layer was concentrated under reduced pressure
- custompurified by C18 reversed-phase HPLC