反应 #452480

ord-2e3029fcef974cf897be40ffa1ed8faf

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with dichloromethane (3×100 ml)
  2. 2
    萃取extracted into dichloromethane (3×100 ml)
  3. 3
    干燥dried (MgSO4)
  4. 4
    其他then evaporated in vacuo
  5. 5
    其他to give a brown oil
  6. 6
    其他The oil was purified by chromatography [alumina; ethyl acetate-toluene (1:4)]

实验过程

1-(2-aminoethyl)-4-(2-methoxyphenyl)piperazine (9.4 g, 40 mmol) and 2-chloroquinoline (6.5 g, 40 mmol) were heated at 160° C. for 3 h, then at 120° C. for 18 h in a sealed vessel. The resultant brown tar was taken up into dilute hydrochloric acid (300 ml), washed with dichloromethane (3×100 ml) basified with sodium hydroxide, extracted into dichloromethane (3×100 ml), dried (MgSO4) then evaporated in vacuo to give a brown oil. The oil was purified by chromatography [alumina; ethyl acetate-toluene (1:4)] to give the product (1.8 g) as a clear oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06127357uspto-grants-2000_10