反応 #5034

ord-461d95d8d5924dfa90fb02af4201c163

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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