HRID1708473

反应详情

EQUATION

反应方程式

HRID 1708473 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 tetrahydrofuran at room temperature is rapidly added 23.63 g of a 1.0M solution of lithium bis(trimethyl- silyl)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

  1. additionis rapidly added in one portion
  2. temperaturethe reaction mixture heated
  3. temperatureat reflux for 48 hours
  4. concentrationthe reaction mixture is concentrated in vacuo to a residue which
  5. customis purified by chromatography on silica gel
  6. washby eluting with 1:3 ethyl acetate-hexanes