HRID1438315
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
To a solution of 1-(6-methoxy-pyridin-3-yl)-ethanol (14.3 g, 93.5 mmol) in anhydrous THF was added triethylamine (32.3 mL), followed by MsCl (8.6 mL, 112 mmol). The resulting mixture was stirred at room temperature for 15 hours before it was filtered through a pad of celite. The filtrate was concentrated in vacuo and the residue was purified by flash column chromatography to afford the desired product (4.7 g, 37% yield). 1H NMR (300 MHz, CDCl3): δ 3.94 (s, 3H), 5.20-5.23 (m, 1H), 5.61-5.67 (m, 1H), 6.60-6.78 (m, 2H), 7.67-7.72 (m, 1H), 8.12 (s, 1H).
WORKUP
后处理
- filtrationwas filtered through a pad of celite
- concentrationThe filtrate was concentrated in vacuo
- customthe residue was purified by flash column chromatography