HRID1727208

反应详情

EQUATION

反应方程式

HRID 1727208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-acetyl-4-{[(4-chlorophenyl)methyl]oxy}piperidine (Preparation 99, 11 g, 41.1 mmol) in methanol (50 ml) and sodium hydroxide solution (5 M, 30 ml) were refluxed on a steam bath for 10 h. After cooling, methanol was removed and the remaining solution was extracted with petroleum ether (40-60, 3×30 ml). The organic extracts were dried (Na2SO4) and concentrated in vacuo to give an white solid (5.8 g, 62%). A portion was recrystallised from petroleum ether to give needle crystals (3 g).

WORKUP

后处理

  1. temperatureAfter cooling
  2. custommethanol was removed
  3. extractionthe remaining solution was extracted with petroleum ether (40-60, 3×30 ml)
  4. dry with materialThe organic extracts were dried (Na2SO4)
  5. concentrationconcentrated in vacuo