Реакция #5034

ord-461d95d8d5924dfa90fb02af4201c163

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05242918uspto-grants-1993_09