反应详情

温度

170 °C

6-Aminonicotinic acid (10 g., 0.072 mol) [Berichte, 26, 2187, (1893)], methyl 4-oxotetrahydro-thiophene-3-carboxylate (28 g., 0.175 mol) [Monats, Chem., 104, 1520(1973)] and p-toluenesulfonic acid monohydrate (1.0 g) are thoroughly mixed and heated at 170° C. under nitrogen for 75 minutes. The distillate is collected in a Dean-Stark trap. The residue is cooled, tritrated with boiling chloroform and filtered to give the product as a yellow powder (11.3 g.). Recrystallization from dimethylformamide gives an analytical sample mp 314°-315° C. (dec).

1. distillationThe distillate is collected in a Dean-Stark trap
2. temperatureThe residue is cooled
3. filtrationfiltered