HRID486623

反应详情

EQUATION

反应方程式

HRID 486623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.0 g of 2-butyl-6-(1H-tetrazol-5-yl)-4(1H)-quinazolinone, 2.2 g of 5-bromo-1-pentene and 2 ml of N,N-diisopropylethylamine in 50 ml of tetrahydrofuran is refluxed for 24 hours. The volatiles are evaporated in vacuo to a residue which is partitioned between chloroform and water. The organic layer is dried over MgSO4, filtered and evaporated in vacuo to a residue which is purified by column chromatography on silica gel by elution with 3:2 ethyl acetate-hexanes to give a residue which crystallizes from ethyl acetate-hexanes to give 2.0 g of the desired product as a solid, m.p. 130° C.

WORKUP

后处理

  1. temperatureis refluxed for 24 hours
  2. customThe volatiles are evaporated in vacuo to a residue which
  3. customis partitioned between chloroform and water
  4. dry with materialThe organic layer is dried over MgSO4
  5. filtrationfiltered
  6. customevaporated in vacuo to a residue which
  7. customis purified by column chromatography on silica gel by elution with 3:2 ethyl acetate-hexanes
  8. customto give a residue which
  9. customcrystallizes from ethyl acetate-hexanes