Reaktion #73435

ord-3977ce71efee440385264c98363f3da1

Reaktionsbedingungen

Temperatur
79°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction is cooled to room temperature
  2. 2
    WaschenThe organic layer is washed with 500 mL of water
  3. 3
    Sonstigeto remove the acid
  4. 4
    TrocknenThe organic layer is dried (sodium sulfate)
  5. 5
    Einengenconcentrated to an oil (352 mg)

Vorschrift

(5-Cyclopropyl-isoxazol-3-yl)-carbamic acid phenyl ester (0.25 g, 1.024 mmol) is dissolved in AcOH (7.31 mL) and NCS (0.205 g, 1.53 mmol) is added and the reaction is heated to 79° C. for 2 hours. The reaction is cooled to room temperature and diluted with water and ethyl acetate. The organic layer is washed with 500 mL of water to remove the acid. The organic layer is dried (sodium sulfate) and concentrated to an oil (352 mg) to obtain the title compound that is used without further purification. MS (ESI) m/z 279.00 (M+1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541432B2uspto-grants-2013_09