反应 #44316

ord-5f8e5d07e27c4cbb8e72a0fb83256796

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the solution heated
  2. 2
    温度at reflux under Dean-Stark conditions for two days
  3. 3
    其他The solvent was removed
  4. 4
    其他the residue purified by silica column chromatography
  5. 5
    洗涤eluting with 25-40% ethyl acetate in hexane

实验过程

To a solution of N-BOC-1,4-diaminobutane (8.324 g, 0.044 mol) in dry toluene (50 ml) was added maleic anhydride (4.336 g, 0.044 mol) and the solution heated at reflux under Dean-Stark conditions for two days. The solvent was removed and the residue purified by silica column chromatography eluting with 25-40% ethyl acetate in hexane to give the title compound, 1.461 g, 12%, as a white solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07736635B2uspto-grants-2010_06