to the preparation of diazomethane via N-nitroso-N-methyl~ rea.~ The final step proceeds smoothly at room temperature, but no matter whether it is carried out in the presence or absence of an organic solvent, hexamethyldisiloxane is formed as a side product. In a typical preparation, 0.119 mole of N-nitroso-N-trimethylsilylmethylurea was suspended in 87 ml of benzene, and 41 ml of 20% KOH solution was added. The mixture was stirred rapidly ...