Reaktion #53339

ord-2801449e76a54039a62ffd7aa20d7690

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated
  2. 2
    SonstigeThe residue was purified
  3. 3
    Temperaturby refluxing in ethanol

Vorschrift

A mixture of 1.0 g (3.07 mmol) of (±)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine, 25 ml of dry dichloromethane and 0.62 g (5.88 mmol of 2-chloroethyl isocyanate was stirred at room temperature for 24 h, then concentrated. The residue was purified by refluxing in ethanol to yield 1.25 g (94%) of the title compound, Mp.: 222-223° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858605B2uspto-grants-2005_02