HRID583062
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
- -50 °C
PROCEDURE
实验过程
2 Fluoronitrobenzene (20.0 g, 0.142 mol) was dissolved in dry tetrahydrofuran (400 ml) and cooled to -50° C. Vinylmagnesium chloride (288 ml, 15% wt/vol) was added at -45° C. and stirred at this temperature for one hour. Poured onto saturated ammonium chloride (600 ml). Separated and aqueous extracted with diethyl ether (2×200 ml). Dried (MgSO4), filtered and concentrated in vacuo to yield a dark oil which was purified by column chromatography on silica using toluene as mobile phase. Fractions concentrated to yield a crystalline solid.
WORKUP
后处理
- customSeparated
- extractionaqueous extracted with diethyl ether (2×200 ml)
- dry with materialDried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto yield a dark oil which
- customwas purified by column chromatography on silica
- concentrationFractions concentrated
- customto yield a crystalline solid