Reaktion #42035

Reaktionsgleichung

ethyl 4-(bromomethyl)-3-trifluoromethylbenzoate

trimethyl phosphite

toluene

→

objective compound

ethyl 4-(dimethoxyphosphorylmethyl)-3-trifluoromethylbenzoate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturat reflux for 4 hours under an argon atmosphere
3. 3
   SonstigeAfter the completion of the reaction
4. 4
   Sonstigefollowed by azeotropic removal of trimethyl phosphite
5. 5
   SonstigeThe residue was purified by silica gel column chromatography

Vorschrift

6.20 g of ethyl 4-(bromomethyl)-3-trifluoromethylbenzoate (Reference Example 2 (step 2)) was dissolved in 12 ml of trimethyl phosphite and the mixture was heated at reflux for 4 hours under an argon atmosphere. After the completion of the reaction, the operation of adding of toluene to the residue, followed by azeotropic removal of trimethyl phosphite was repeated three times. The residue was purified by silica gel column chromatography to obtain 4.96 g of the objective compound as a yellow oily product.

Quelle