反应 #452474

ord-c5756552bbd3491fba645fbf4c5e7481

反应方程式

Nc1cccc2c1OCCO2
product
Nc1cccc2c1OCCO2
2,3-Dihydro-1,4-benzodioxin-5-amine
Cl.ClCCNCCCl
bis(2-chloroethyl)amine hydrochloride
c1cc2c(c(N3CCNCC3)c1)OCCO2
product
收率 90.8%
c1cc2c(c(N3CCNCC3)c1)OCCO2
1-(2,3-Dihydro-1,4-benzodioxin-5-yl)piperazine
收率 90.8%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度under reflux for 24 h
  2. 2
    其他evaporated in vacuo
  3. 3
    workup.DISSOLUTIONThe white solid was dissolved in aqueous sodium hydroxide (100 ml)
  4. 4
    萃取extracted into ethyl acetate (3×50 ml)
  5. 5
    干燥The extracts were dried (MgSO4)
  6. 6
    其他evaporated in vacuo

实验过程

The solution of the product of example 13 (1.50 g, 0.010 mol) and bis(2-chloroethyl)amine hydrochloride (1.77 g 0.01 mol) in chlorobenzene (20 ml) was heated under reflux for 24 h, cooled to room temperature and evaporated in vacuo. The white solid was dissolved in aqueous sodium hydroxide (100 ml) and extracted into ethyl acetate (3×50 ml). The extracts were dried (MgSO4) and evaporated in vacuo to give the product (2.00 g).

来源

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