反应详情

4.982 g of 97% ortho-nitrosotoluene (41.12 mmol) were dissolved in 20 ml of methylene chloride at room temperature and 5.93 g of 98% methane sulfonic acid (61.7 mmol = molar ratio of 1:1.5) added thereto in the course of 2 minutes. Stirring was continued for one-half hour at room temperature and subsequently the dark brown, clear solution sprayed into water of 30° C. under a vacuum, whereby the methylene chloride was distilled off simultaneously. By means of filtration, it was possible to obtain 4.85 g = 97% of theoretical, of N-(2-methylphenyl)-N-(3-methyl-4-nitrosophenyl)-hydroxylamine in the form of a light yellow powder.

1. customin the course of 2 minutes
2. waitwas continued for one-half hour at room temperature
3. distillationwas distilled off simultaneously
4. filtrationBy means of filtration, it