Reaktion #531650

Reaktionsgleichung

2,6-Dimethylbenzoyl isocyanate

6-(4-chlorophenylthio)-3-aminopyridine

→

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

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeSolvent was removed in vacuo
2. 2
   workup.ADDITIONThe mixture was passed over a column of silica gel with a 1:1 mixture of toluene-ethyl acetate
3. 3
   Sonstigethe product (Rf ≅0.7) separated
4. 4
   Sonstigecrystallized from ethyl acetate-hexanes, yield 1.1 grams, m.p. 159°-160° C.

Vorschrift

2,6-Dimethylbenzoyl isocyanate (1.61 grams; 0.01 mole) and 6-(4-chlorophenylthio)-3-aminopyridine (2.36 grams; 0.01 mole) were mixed in 50 ml. of ethyl acetate and stirred at room temperature for 12 hours. Solvent was removed in vacuo. TLC showed four spots. The mixture was passed over a column of silica gel with a 1:1 mixture of toluene-ethyl acetate and the product (Rf ≅0.7) separated and crystallized from ethyl acetate-hexanes, yield 1.1 grams, m.p. 159°-160° C.

Quelle