反应详情

4-[[(Dimethylamino)methylene]amino]-3-pyridinol (1.65 g) was refluxed for 1 hour in 20 ml of benzene containing 1.10 g of Et3N and 1.10 g of N,N-dimethylcarbamyl chloride. At the end of this time, the reaction mixture was applied directly to a silica column and eluted with 5% Et3N/ethyl acetate. Concentration of the product-containing fractions gave 2.05 g of chromatographically pure product which was distilled in a bulb to bulb apparatus (oven temperature=175° C.) to give analytically pure material, m.p. 64°-66° C.

1. washeluted with 5% Et3N/ethyl acetate
2. customConcentration of the product-containing fractions gave 2.05 g of chromatographically pure product which
3. distillationwas distilled in a bulb to bulb apparatus (oven temperature=175° C.)
4. customto give analytically pure material, m.p. 64°-66° C.