Reaktion #413875

Reaktionsgleichung

HCl

N-[6-chloro-5-(p-chloro-phenyl)-4-pyrimidinyl]-α,α,α-trifluoro-p-toluenesulfonamide

ethylene glycol

→

N-[5-(p-chlorophenyl)-6-(2-hydroxyethoxy)-4-pyrimidinyl]-α,α,α-trifluoro-p-toluenesulfonamide

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to room temperature
2. 2
   Waschenthe organic extracts were washed with water
3. 3
   Sonstigedried
4. 4
   Sonstigeevaporated under reduced pressure
5. 5
   SonstigeThe precipitate remaining behind was recrystallized from CH2Cl2, isopropyl ether and n-hexane

Vorschrift

A solution of 0.046 g of Na in 1.5 ml of absolute ethylene glycol was treated with 0.216 g of N-[6-chloro-5-(p-chloro-phenyl)-4-pyrimidinyl]-α,α,α-trifluoro-p-toluenesulfonamide with the exclusion of moisture and heated at 100° C. for 3 hours, thereafter cooled to room temperature and treated with 2.3 ml of 1N HCl. The mixture was taken up in ethyl acetate, the organic extracts were washed with water, dried and evaporated under reduced pressure. The precipitate remaining behind was recrystallized from CH2Cl2, isopropyl ether and n-hexane and yielded N-[5-(p-chlorophenyl)-6-(2-hydroxyethoxy)-4-pyrimidinyl]-α,α,α-trifluoro-p-toluenesulfonamide, melting point 160°-162° C.

Quelle