تفاعل #5034

ord-461d95d8d5924dfa90fb02af4201c163

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto reflux for 1 hour, whereafter it
  2. 2
    ترشيحfiltered
  3. 3
    أخرىThe filtrate was evaporated
  4. 4
    workup.DISSOLUTIONthe residue dissolved in methanol (10 ml)
  5. 5
    درجة الحرارةrefluxed for 10 min
  6. 6
    أخرىEvaporation of the solvent
  7. 7
    workup.WAITleft the crude title compound as a solid, M.p. 270° C.

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05242918uspto-grants-1993_09