Reacción #5034

ord-461d95d8d5924dfa90fb02af4201c163

Ecuación de reacción

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

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05242918uspto-grants-1993_09