Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 58443665 | HCID 58443665 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86657769 | HCID 86657769 | 104.2% |
Reaction Steps
To a solution of 3-(2,4,6-trichloro-phenyl)-propionaldehyde (0.45 g, 1.8 mmol) in methanol (5 ml), triethylamine (0.4 ml, 2.8 mmol) followed by O-methylhydroxylamine-hydrochloride (0.24 g, 2.8 mmol) was added and the mixture was heated at 60° C. for 2 hours. When the TLC confirmed the completion of the reaction, the reaction mass was allowed to attain ambient temperature and quenched with water and methanol was removed with a rotavapor. The resulting aqueous solution was extracted with ethyl acetate (3×30 ml). The combined ethyl acetate layers were washed with water and dried over sodium sulfate before complete evaporation of the solvents to give the crude mass. The resulting crude mass was purified over column chromatography (silica gel 60-120 mesh, 1% ethyl acetate in hexane) to afford 3-(2,4,6-trichloro-phenyl)-propionaldehyde O-methyl-oxime (0.5 g, 80%)
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-2a922ae5cf3b4d83a702e0cc01ad2fb7 |
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| Source note | uspto-grants-2012_09 |
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