Réaction #48024

ord-1911c6d38c2143cabee43681d994bac6

Conditions de réaction

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

Traitement

  1. 1
    Autrekept in a refrigerator overnight
  2. 2
    Extractionthe mixture was extracted with ethyl acetate (4×250 ml)
  3. 3
    LavageThe combined organic phases were washed with water
  4. 4
    Autredried
  5. 5
    workup.ADDITIONtreated with charcoal
  6. 6
    Autreevaporated to dryness

Mode opératoire

50 g (0.245 mol) of m-trifluoromethyl-benzamidoxime and 33.7 g (0.6 mol) of potassium hydroxide was dissolved in a mixture of dimethyl sulphoxide and 170 ml of water, and the mixture was cooled to 0° C. 48 ml (0.6 mol) of epichlorohydrine was added, and the reaction mixture was stirred at 0° C. for 5 hours, then kept in a refrigerator overnight. Next day 250 ml of water was added, and the mixture was extracted with ethyl acetate (4×250 ml). The combined organic phases were washed with water, dried, treated with charcoal and evaporated to dryness, to yield m-trifluoromethyl-N-(2,3-epoxypropoxy)-benzamidine, as a colorless oil.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07745465B2uspto-grants-2010_06