反应 #83898

ord-15115cea8d9044eb8ed145a002f54995

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 3.5 hours
  3. 3
    过滤The insolubles were filtered
  4. 4
    其他The solvent was removed at reduced pressure
  5. 5
    其他the residue was purified by silica gel column chromatography

实验过程

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (6.44 g, 29.1 mmole), K2CO3 (6.4 g, 46 mmol), N-(3-bromopropyl)phthalimide (8.4 g, 31 mmol) in acetonitrile (150 ml) was heated at reflux for 3.5 hours. The insolubles were filtered. The solvent was removed at reduced pressure and the residue was purified by silica gel column chromatography to give N-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propyl]phthalimide as a white solid. Recrystallization from ethanol yielded 9.8 g (83%) of off-white crystals, m.p.=129°-130° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05624927uspto-grants-1997_04