Réaction #1757083

ord-58b442b1ed1944798bbc2c66f53360ab

Conditions de réaction

Température
0°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe temperature below 15° C
  2. 2
    workup.STIRRINGThe reaction mixture was then stirred at room temperature overnight
  3. 3
    LavageThe reaction mixture was washed with water (2×100 mL)
  4. 4
    Autrefollowed by evaporation to an oil

Mode opératoire

4-(Methylthio)phenol (28 g) and dichloromethane (100 mL) were charged to a vessel. The vessel was cooled to approximately 0° C. 1-Chloro-2-methylpropyl chloroformate (14 mL) was added. A solution of 4-methylmorpholine (24 g) in dichloromethane (100 mL) was then slowed added using an addition funnel, keeping the temperature below 15° C. The reaction mixture was then stirred at approximately 0° C. for 10 minutes. The reaction mixture was then stirred at room temperature overnight. The reaction mixture was washed with water (2×100 mL) followed by evaporation to an oil. Fifty-four grams (54 g) of the title compound D4 was obtained.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07989641B2uspto-grants-2011_08