HRID1639075
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
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
- temperaturewas heated
- temperatureat reflux for 48 hr
- customThe resulting reaction mixture
- customto stand in a refrigerator overnight
- filtrationfiltered
- additionThe filtrate was treated with ethereal hydrogen chloride
- customprecipitated with ether
- filtrationUpon filtering
- customa white crystalline solid formed which
- customThis was recrystallized with isopropanol yielding 36 g of the free base, m.p. 100°-101.5° C.