反应 #562135

ord-cf4f10a2c03f439caa2b6f9546401973

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux for 16 h
  2. 2
    浓缩The mixture was concentrated
  3. 3
    其他the residue was purified by column chromatography (80 g ISCO column
  4. 4
    洗涤eluting with methylene chloride

实验过程

Piperazinone (2.2 g, 22 mmol), 2-(2-chloroethyl)pyridine hydrochloride (3.9 g, 22 mmol) and i-Pr2NEt (5.67 g, 7.6 mL, 44 mmol) were heated at reflux for 16 h. The mixture was concentrated, and the residue was purified by column chromatography (80 g ISCO column eluting with methylene chloride and a 10:1 methanol/ammonium hydroxide mixture; gradient 100% methylene chloride to 90% methylene chloride) to provide the title compound (1.5 g, 33%) as a yellow solid; ESI MS m/z 206 [M+H]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08637501B2uspto-grants-2014_01