HRID1460258

反应详情

EQUATION

反应方程式

HRID 1460258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9.1 g (0.03 mole) of [α,α-bis(p-fluorophenyl)]-4-piperidinemethanol and 8.6 g (0.03 mole) of 4-(3-chloropropoxy)-3-methoxybenzeneacetic acid ethyl ester, 10.6 g (0.1 mole) of anhydrous sodium carbonate and 0.5 g of potassium iode in 150 ml of dimethylformamide was heated on a steambath for 20 hr. The mixture was concentrated under reduced pressure and the residue was partitioned between water and benzene. The benzene layer was washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give an off-white solid which was recrystallized from isopropyl ether/2-propanol. The yield of the title compound was 12.7 g (77%), mp 110°-112° C.

WORKUP

后处理

  1. temperaturewas heated on a steambath for 20 hr
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customthe residue was partitioned between water and benzene
  4. washThe benzene layer was washed with water and saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customto give an off-white solid which
  8. customwas recrystallized from isopropyl ether/2-propanol