4-Nitrosophenol → 5990-80-7

Participants

Reaction Conditions

Reaction Steps

A, is slowly added dropwise in order to achieve a permanent exothermal reaction. The solvent is stirred under reflux at ambient pressure. After termination of said exothermal reaction, the reaction mixture is cooled down to 2° C., and subsequently, 155.5 g (872 mmol) methyl triethoxysilane in 160 ml dry diethyl ether is added; the temperature should not substantially exceed 15° C. After termination of the substitution reaction, stirring is continued over night at ambient temperature. Subsequently, about 200 ml n-heptane is added to obtain a precipitation of the magnesium salts. The magnesium salts are separated by filtration, 5.4 g (0.44 mmol) 4-nitrosophenol is added to the filtrate, the solvent is removed in a rotary evaporator, and the residue is subjected to a fractionating distillation under vacuum. 72.5 g (307 mmol) of the product was obtained.

Provenance & Evidence