反应详情

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.

1. customThe ethyl acetate was removed in vacuo
2. additionThe reaction mixture was then poured over a silica column with ethyl acetate
3. customthe major spot collected
4. customIt was crystallized from ethyl acetate-hexanes, yield 1.5 g