HRID420433
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
Step-1: To the stirred solution of 2-chloroacetamidoxime (1.0 g, 9.2 mmol, prepared as per the procedure given in PCT/US02/22897) in toluene (15 ml) was added nicotinyl chloride (1.37 g, 9.67 mmol) and heated at 110° C. for 4 hr. The reaction mixture was diluted with ethyl acetate (50 ml) and washed with aqueous saturated sodium bicarbonate solution (2×25). Organic layer was evaporated under vacuum to yield the crude product. The crude product was purified using silica gel column chromatography (15% Acetone-Hexane) to give 2-(3-chloromethyl-[1,2,4]-oxadiazole-5-yl)-pyridine in 55% (0.550 g) yield. MS: m/z: 196.7 (M+1).
WORKUP
后处理
- washwashed with aqueous saturated sodium bicarbonate solution (2×25)
- customOrganic layer was evaporated under vacuum
- customto yield the crude product
- customThe crude product was purified