Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 20378192 | HCID 20378192 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 74042289 | HCID 74042289 | 100% |
Reaction Steps
A mixture of 4.0 g (0.1 mole) of powdered sodium hydroxide, 13.9 g (0.2 mole) of hydroxylamine hydrochloride, and 27.4 g (0.1 mole) of N-methyl-N-(2-benzoyl-4-chlorophenyl)formamide in 200 ml of ethanol was refluxed for 3 days. About one-half of the ethanol was distilled off and the reaction mixture was poured into 500 ml of water and then extracted with three 100-ml portions of methylene chloride. The extracts were combined, washed with water, dried (MgSO4) and evaporated to dryness under reduced pressure to give 26 g (100%) of a light yellow glass: 1H nmr (DMSO-d6) partial: δ 2.74 ppm (d, J=5 Hz) and δ 2.94 ppm (d, J=5) for CH3 split by NH; δ 11.26 ppm (45% ) and 11.53 ppm (55%) for =NOH (on addition of D2O, the splitting of the methyl peaks is lost).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04182760 |
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| Source dataset | uspto-grants-1980_01 |
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| ORD ID | ord-16b9479ddb3e4f6e8cc51c5a2f417913 |
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| Source note | uspto-grants-1980_01 |
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