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 suspension of 4.49 g of 2-Butyl-6-ethenyl-4(1H)-quinazolinone in 70 ml of dry tetrabydrofuran at room temperature is rapidly added 23.63 9 of a 1.0M solution of lithium bis(trimethylsilyl)amide in tetrahydrofuran. After stirring for 20 minutes at room temperature 21.94 g of 5-(4'-(bromomethyl)-[1,1'-biphenyl]-2-yl]-1-(triphenylmethyl)-1H-tetrazole is rapidly added in one portion and the reaction mixture heated at reflux for 48 hours. After cooling to room temperature, the reaction mixture is concentrated in vacuo to a residue which is purified by chromatography on silica gel by eluting with 1:3 ethyl acetate-hexanes to give 9.58 g of the desired product as a yellow solid. FAB MASS SPEC 705 (M+H)
WORKUP
后处理
- additionis rapidly added in one portion
- temperaturethe reaction mixture heated
- temperatureat reflux for 48 hours
- concentrationthe reaction mixture is concentrated in vacuo to a residue which
- customis purified by chromatography on silica gel
- washby eluting with 1:3 ethyl acetate-hexanes