反应详情

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.

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