反应 #1176

ord-64836a6fca744252ac2345f2b4e4762d

反应方程式

Oc1ccc(Oc2ccccc2)cc1
4-phenoxyphenol
Cl.ClCCN1CCCC1
1-(2-chloroethyl)-pyrrolidine HCl
CCOCC
Et2O
O
water
c1ccc(Oc2ccc(OCCN3CCCC3)cc2)cc1
brown oil
收率 92.9%
c1ccc(Oc2ccc(OCCN3CCCC3)cc2)cc1
1-[2-(4-phenoxyphenoxy)ethyl]pyrrolidine
收率 92.9%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The solution was cooled
  2. 2
    洗涤the ether layer washed with water and brine
  3. 3
    干燥dried over Na2SO4
  4. 4
    浓缩concentrated in vacuo

实验过程

A solution of 4-phenoxyphenol (0.56 g, 3.0 mmol), 1-(2-chloroethyl)-pyrrolidine HCl (0.51 g, 3.0 mmol) and powdered K2 CO3 (1.2 g, 8.7 mmol) in 30 mL DMF was stirred at 80°-90° C. for 15 hours. The solution was cooled, poured into Et2O and water and the ether layer washed with water and brine, dried over Na2SO4 and concentrated in vacuo to give 0.79 g of a brown oil. The crude product was flashed chromatographed on silica gel using a gradient of 2:1 hexane/EtOAc to 100% EtOAc to provide the title compound (0.65 g, 76.5%) as a light yellow oil:

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723492uspto-grants-1998_03