Water → HCID 69413636, compound

Participants

Reaction Steps

400 g of 2-acetylthiophene, 314 g of methyl cyanoacetate and 48.8 g of ammonium acetate were dissolved in a mixture of 153 ml of acetic acid and 1.5 l of toluene, and the resulting reaction solution was refluxed under heating for 8 hours while water was removed. The reaction solution was washed sufficiently with water and then dried over anhydrous magnesium sulfate. Removal of the solvent by distillation was followed by vacuum distillation (b.p. 110°-140° C./0.05 mmHg) to give 263.4 g of methyl 2-cyano-3-(2-thienyl)crotonate. (Yield 40%)

Provenance & Evidence