Reaktion #531647

Reaktionsgleichung

2,6-Dichlorobenzoyl isocyanate

6-(4-chlorophenylthio)-3-aminopyridine

→

1-(2,6-DICHLOROBENZOYL)-3-(6-(4-CHLOROPHENYLTHIO)-3-PYRIDINYL)UREA

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe ethyl acetate was removed in vacuo
2. 2
   workup.ADDITIONThe reaction mixture was then poured over a silica column with ethyl acetate
3. 3
   Sonstigethe major spot collected
4. 4
   SonstigeIt was crystallized from ethyl acetate-hexanes, yield 1.5 g

Vorschrift

2,6-Dichlorobenzoyl isocyanate (2.16 grams; 0.01 mole) and 6-(4-chlorophenylthio)-3-aminopyridine (2.37 grams; 0.01 mole) were mixed in dry ethyl acetate and stirred for 4 hours. The ethyl acetate was removed in vacuo. TLC showed a 3-spot mixture. The reaction mixture was then poured over a silica column with ethyl acetate, and the major spot collected. It was crystallized from ethyl acetate-hexanes, yield 1.5 g., m.p. 160°-162° C.

Quelle