Reaktion #49607

ord-5ac828f8d5b84688b668aa8943cfeb3b

Reaktionsgleichung

Cl.NCCCOc1cc(I)c2c(c1Cl)CNC2=O
4-Chloro-5-(3-aminopropoxy)-7-iodoisoindolinone hydrochloride
CCN(CC)CC
triethylamine
CCN=C=O
ethyl isocyanate
CCNC(=O)NCCCOc1cc(I)c2c(c1Cl)CNC2=O
4-chloro-5-[3-(ethylcarbamoylamino)propoxy]-7-iodoisoindolinone
Ausbeute 93.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe residue was purified by slurry

Vorschrift

4-Chloro-5-(3-aminopropoxy)-7-iodoisoindolinone hydrochloride (100 mg, 0.248 mmol) was suspended in dichloromethane (3.0 mL), and the suspension was added with triethylamine (0.104 mL, 0.744 mmol) and ethyl isocyanate (0.029 mL, 0.372 mmol), followed by stirring at room temperature for 13 hours. The solvent was evaported under reduced pressure and the residue was purified by slurry using water and acetonitrile to obtain 4-chloro-5-[3-(ethylcarbamoylamino)propoxy]-7-iodoisoindolinone (100 mg, yield 93%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745641B2uspto-grants-2010_06