Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Benzoic acid, 2-nitroso-, methyl ester | HCID 10877472 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22756872 | HCID 22756872 | 44% |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04129740 |
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| Source dataset | uspto-grants-1978_12 |
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| ORD ID | ord-1ee9b8b463bc44748b9f191881ff1b52 |
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| Source note | uspto-grants-1978_12 |
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