반응 #1735421

ord-19dd2e371e464c27bc6e1f55fee1a850

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to reflux for 1 hour, whereafter it
  2. 2
    여과filtered
  3. 3
    기타The filtrate was evaporated
  4. 4
    workup.DISSOLUTIONthe residue dissolved in methanol (10 ml)
  5. 5
    온도refluxed for 10 min
  6. 6
    기타Evaporation of the solvent
  7. 7
    workup.WAITleft the crude title compound as a solid, M.p. 270° C.

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05436250uspto-grants-1995_07