Carbohydrazides (carboxylic hydrazides) are typically made via hydrazinolysis of carboxylic acid esters in alcoholic solutions. Herein, we present a method for the synthesis of thiophene carbohydrazides with yields more than 90% and good purity via the chemical reaction of activated esters or amides with hydrazine. This novel technique was used to synthesis and analyze a variety of heteroaryl-, aryl-, and aralkyl-substituted carbohydrazides.