Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 58231449 | HCID 58231449 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86657768 | HCID 86657768 | 97.8% |
Reaction Steps
To a stirred solution of 4-(2,4,6-trichloro-phenyl)-butan-2-one (0.9 g, 3.57 mmol) in methanol (5 ml), was added triethylamine (0.73 ml, 5.3 mmol) and O-methyl-hydroxylamine hydrochloride (0.447 g, 5.3 mmol). The reaction mixture was heated at a temperature of 60° C. for 3 hours. When the TLC confirmed the completion of the reaction, the reaction mass was allowed to attain ambient temperature. After the reaction mixture was diluted with water and methanol was evaporated off, the aqueous layer was extracted with ethyl acetate (3×30 ml). The combined ethyl acetate layers were washed with water followed by brine solution and dried over sodium sulfate before complete evaporation of the solvents to give 4-(2,4,6-trichloro-phenyl)-butan-2-one O-methyl-oxime (0.980 g) crude, which was taken up for reduction without any further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08258169B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-70565df18f0b4928a0513370a993db41 |
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| Source note | uspto-grants-2012_09 |
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