反应 #1797556

ord-4b1be3494c0d4e5c8e213bc2967a5241

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Thereafter, the reaction mixture is evaporated to dryness
  2. 2
    其他to yield approximately 200 mg of crude material, which
  3. 3
    其他is purified by chromatography on basic aluminum oxide (eluent: dichloromethane)

实验过程

90 mg of 7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-azepan-2-one (compound B1) are dissolved in 10 ml of toluene under an atmosphere of dry nitrogen. Subsequently, 144 mg of Lawesson's reagent are added and the solution is heated at 100° C. for 17 hours. Thereafter, the reaction mixture is evaporated to dryness to yield approximately 200 mg of crude material, which is purified by chromatography on basic aluminum oxide (eluent: dichloromethane) to afford 71 mg of the title compound as a light yellow, waxy solid. ESI-MS: 351.2 (MH+). TLC: Rf=0.53 (dichloromethane/ethanol 10:1 parts by volume).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07790710B2uspto-grants-2010_09