反应 #4930

ord-899dfc4eb3d343fca6a7503b6a131990

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to evaporate
  2. 2
    其他the residue was partitioned between chloroform and dilute sodium hydroxide
  3. 3
    浓缩The chloroform layer was concentrated
  4. 4
    workup.DISSOLUTIONthe residue, the free base of the title compound, was dissolved in isopropyl alcohol
  5. 5
    其他reacted with hydrogen chloride

实验过程

A solution of 1.5 g (0.0058 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one in 20 ml of dimethylamine was stirred at 25° C. in a sealed container for 72 hr. The excess dimethylamine was allowed to evaporate and the residue was partitioned between chloroform and dilute sodium hydroxide. The chloroform layer was concentrated and the residue, the free base of the title compound, was dissolved in isopropyl alcohol and reacted with hydrogen chloride. The resulting hydrochloride salt weighted 1.5 g (77%), m.p.>250° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04727152uspto-grants-1988_02