(Trimethylsilyl) ethoxyacetylene, a stable and easy-handling reagent, serves as an excellent dehydrating agent for the synthesis of carboxylic anhydrides and amides from the corresponding carboxylic acids. By means of this reagent, various types of acid-sensitive carboxylic anhydrides and amides were obtained almost in quantitative yields. Twenty-two examples of carboxylic anhydrides and 12 examples of amides were presented.