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
The tetrazole (a) (3.0 g; 0. 015 moles) was taken up in acetonitrile (50 mL) containing two equivalents of triethylamine (3.0 g; 0.030 moles). The suspension was heated to reflux and then treated with 1-bromododecane (3.7 g; 0.015 moles) dropwise for several minutes. The solution was refluxed for 16 hours, cooled to room temperature, and the solvent removed in vacuo. The residue was triturated with ethyl acetate, filtered, and concentration of the filtrate in vacuo leaving a maroon-colored liquid. The 2-isomer was obtained by dissolving the crude product in 50% hexane/50% ethyl acetate and removing the impurities, including the 1-regioisomer, by silica gel chromatography. Yield: 2.0 g (41%).
WORKUP
后处理
- temperatureThe suspension was heated
- temperatureto reflux
- temperatureThe solution was refluxed for 16 hours
- customthe solvent removed in vacuo
- customThe residue was triturated with ethyl acetate
- filtrationfiltered
- customconcentration of the filtrate in vacuo leaving a maroon-colored liquid
- customThe 2-isomer was obtained
- customremoving the impurities