HRID2164744

反应详情

EQUATION

反应方程式

HRID 2164744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-amino-4-[3-(1-piperidinylmethyl)phenoxy]-2-butanol (1.39 g) and 5-bromo-1-methyl-1H-tetrazole (0.82 g) in absolute ethanol (10 ml) was heated in an autoclave at 125° for 18 h. The solution was evaporated and the residue dissolved in 1M hydrochloric acid (25 ml). The acidic solution was washed with ethyl acetate, basified with excess sodium carbonate and extracted with ethyl acetate. The extract was dried and evaporated to leave a solid which was triturated with dry diethyl ether to give a white solid (1.0 g). This solid was recrystallised from methyl acetate-light petroleum (b.p. 60°-80°) to give the title compound (0.6 g) as white crystals, m.p. 138°-9°.

WORKUP

后处理

  1. customThe solution was evaporated
  2. dissolutionthe residue dissolved in 1M hydrochloric acid (25 ml)
  3. washThe acidic solution was washed with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. customThe extract was dried
  6. customevaporated
  7. customto leave a solid which
  8. customwas triturated with dry diethyl ether