Abstract Trimethylsilyldiazomethane was prepared by the action of aqueous KOH on nitroso- N-(trimethylsilylmethyl) urea. The spectroscopic properties of this stable, greenish-yellow liquid which can be isolated by gas chromatography are discussed. Its reaction with acetic acid gives the expected CH 3 CO 2 CH 2 SiMe 3 in addition to Si C cleavage products, CH 3 CO 2 CH 3 and CH 3 CO 2 SiMe 3. Products of the 1, 3-dipolar addition of Me 3 SiCHN ...