HRID2356633
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
Potassium carbonate (82 mg) was added to a solution of (6-cyano-5-methyl-2-pyridinyl)methyl acetate (3.62 g) in methanol (25 ml) and the mixture stirred under argon at ambient temperature for 2 hours. It was concentrated in vacuo to ca. ¼ volume and water (50 ml) added. The mixture was neutralized with 5% acetic acid (1.5 ml) and extracted with dichloromethane (50 ml then 2×25 ml). The combined extracts were washed with brine (25 ml), dried (MgSO4) and concentrated in vacuo. The residue was recrystallised from ether:hexane to afford the title compound (2.26 g, 80%) as a pale buff solid.
WORKUP
后处理
- concentrationIt was concentrated in vacuo to ca. ¼ volume and water (50 ml)
- additionadded
- extractionextracted with dichloromethane (50 ml
- washThe combined extracts were washed with brine (25 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was recrystallised from ether