HRID2115641
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
PROCEDURE
实验过程
A suspension of 3-hydroxypicolinonitrile (3.00 g, 25.0 mmol), which was prepared according to “Synthesis” 316 (1983) and “J. Org. Chem.” 48 1375 (1983), potassium carbonate (5.40 g, 39.1 mmol) and benzyl bromide (5.10 g, 29.8 mmol) in acetone (150 mL) was stirred at room temperature for 20 hrs. The reaction mixture was filtrated and the filtrate was evaporated. The residue was purified by column chromatography on silica gel (ethyl acetate/n-hexane=1/3 to 1/2) followed by recrystallization from ethyl acetate/n-hexane=1/4 to give 3-benzyloxypicolinonitrile as a colorless solid (4.354 g, yield; 83%).
WORKUP
后处理
- customwas prepared
- customaccording to “Synthesis” 316 (1983) and “J
- filtrationThe reaction mixture was filtrated
- customthe filtrate was evaporated
- customThe residue was purified by column chromatography on silica gel (ethyl acetate/n-hexane=1/3 to 1/2)
- customfollowed by recrystallization from ethyl acetate/n-hexane=1/4