Réaction #595335

ord-01901bcf48d84da2958c5005252af0f4

Équation de réaction

Cc1cc(C(N)=O)ccc1F
4-fluoro-3-methylbenzamide
O=C(CCl)CCl
1,3-dichloro-acetone
O=S(=O)(O)O
sulfuric acid
Cc1cc(-c2nc(CCl)co2)ccc1F
4-(Chloromethyl)-2-(4-fluoro-3-methylphenyl)-1,3-oxazole

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreA melt is formed
  2. 2
    workup.STIRRINGstirred at RT overnight
  3. 3
    AutreThe precipitate formed
  4. 4
    Filtrationis filtered off
  5. 5
    Autredried at 40° C. in a vacuum
  6. 6
    Autredrying cabinet overnight

Mode opératoire

2.00 g (12.80 mmol) of 4-fluoro-3-methylbenzamide and 1.79 g (14.08 mmol) of 1,3-dichloro-acetone are stirred at 130° C. for 2 days. A melt is formed. The mixture is then cooled to RT, 3.0 ml of conc. sulfuric acid are added carefully at this temperature and the mixture is stirred for 15 min. The resulting suspension is poured into 20 ml of ice-water and stirred at RT overnight. The precipitate formed is filtered off and dried at 40° C. in a vacuum drying cabinet overnight.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09095582B2uspto-grants-2015_08