Reacción #74007

ord-9e4cccf24b6b4980b14ac92df2305b3c

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroInto a 50-mL round-bottom flask purged
  2. 2
    Temperaturamaintained with an inert atmosphere of nitrogen
  3. 3
    TemperaturaThe resulting solution was heated
  4. 4
    Temperaturato reflux for 40 min
  5. 5
    OtroThe solvent was removed under vacuum

Procedimiento

Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 3-(2-(2-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)ethoxy)ethoxy)propanoic acid (700 mg, 1.99 mmol, 1.00 equiv) in anhydrous DCM (30.0 mL), then oxalyl dichloride (0.7 mL) was added dropwise at room temperature. Two drops of anhydrous DMF were then added. The resulting solution was heated to reflux for 40 min. The solvent was removed under vacuum to yield 750 mg of 3-(2-(2-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)ethoxy)ethoxy)propanoyl chloride as pale yellow oil, which was used directly for the next reaction step without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08541448B2uspto-grants-2013_09