反应 #5034

ord-461d95d8d5924dfa90fb02af4201c163

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to reflux for 1 hour, whereafter it
  2. 2
    过滤filtered
  3. 3
    其他The filtrate was evaporated
  4. 4
    workup.DISSOLUTIONthe residue dissolved in methanol (10 ml)
  5. 5
    温度refluxed for 10 min
  6. 6
    其他Evaporation of the solvent
  7. 7
    workup.WAITleft the crude title compound as a solid, M.p. 270° C.

实验过程

To an ice cooled stirred suspension of 6,7,8,9-tetrahydro-7-methyl-1H-pyrrolo[2,3-f]isoquinoline-2,3-dione (500 mg) in 1,2-dichloroethane (10 ml) was added α-chloroethylchloroformate (0.25 ml). The mixture was then brought to reflux for 1 hour, whereafter it was cooled to room temperature and filtered. The filtrate was evaporated, the residue dissolved in methanol (10 ml) and refluxed for 10 min. Evaporation of the solvent left the crude title compound as a solid, M.p. 270° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05242918uspto-grants-1993_09