HRID1639075

反应详情

EQUATION

反应方程式

HRID 1639075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 35.1 g (0.15 mole) of 1-(o-chlorophenoxy)-2-hydroxybutyl chloride, 32.6 g (0.2 mole) of N-phenylpiperazine and 400 ml of 2-propanol was heated at reflux for 48 hr. The resulting reaction mixture was allowed to stand in a refrigerator overnight and filtered. The filtrate was treated with ethereal hydrogen chloride and precipitated with ether. Upon filtering, a white crystalline solid formed which was dissolved in dilute hydrochloric acid and the mixture was then neutralized with aqueous sodium hydroxide producing a crystalline precipitate. This was recrystallized with isopropanol yielding 36 g of the free base, m.p. 100°-101.5° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 48 hr
  3. customThe resulting reaction mixture
  4. customto stand in a refrigerator overnight
  5. filtrationfiltered
  6. additionThe filtrate was treated with ethereal hydrogen chloride
  7. customprecipitated with ether
  8. filtrationUpon filtering
  9. customa white crystalline solid formed which
  10. customThis was recrystallized with isopropanol yielding 36 g of the free base, m.p. 100°-101.5° C.