Reaktion #5034

ord-461d95d8d5924dfa90fb02af4201c163

Reaktionsgleichung

CN1CCc2c(ccc3c2NC(=O)C3=O)C1
6,7,8,9-tetrahydro-7-methyl-1H-pyrrolo[2,3-f]isoquinoline-2,3-dione
CC(Cl)OC(=O)Cl
α-chloroethylchloroformate
O=C1Nc2c(ccc3c2CCNC3)C1=O
6,7,8,9-tetrahydro-1H-pyrrolo[2,3-f]isoquinoline-2,3-dione

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05242918uspto-grants-1993_09