反应详情

8.2 g (50 mmol) of 2-nitroso-benzoic acid methyl ester were dissolved in 50 ml of methylene chloride and 7.2 g (75 mmol) of methane solufonic acid added thereto at 0° C. Upon addition of the methane sulfonic acid, the green solution turned dark red. During the entire duration of the reaction the temperature of the reaction mixture did not exceed 10° C. After 1 hour (as described in detail in previous Examples), the solution was sprayed onto water under a vacuum and the methylene chloride removed at the same time. By means of filtration it was possible to obtain 3.6 g (44% of theoretical) of N-(2-carbomethoxyphenyl)-N-(3-carbomethoxy-4-nitrosophenyl)-hydroxylamine in the form of a beige powder (decomposition from 85° C. on), the identity of which was ascertained by means of elementary analysis, titration and spectra (NMR, UV, IR).

1. customat 0° C
2. customDuring the entire duration of the reaction the temperature of the reaction mixture
3. customdid not exceed 10° C
4. customthe methylene chloride removed at the same time
5. filtrationBy means of filtration it