HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 68732474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59570280 | HCID 59570280 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 68732474 | HCID 68732474 | 91.2% |
Reaction Steps
To 5 ml of ethanol were added 0.4 g of sodium bicarbonate and 0.33 g of hydroxylamine hydrochloride, and the mixture was heated to reflux for 1 hour. After allowing to cool, 0.67 g of 3,5-dichloro-4-(2,2,2-trifluoro-1-methylethoxy)pyridine-2-carbonitrile at room temperature, and the mixture was stirred for 4 hours, and concentrated. To the residue was added water, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was washed with hexane three times to obtain 0.65 g of 3,5-dichloro-4-(2,2,2-trifluoro-1-methylethoxy)pyridine-2-carboxamide=oxime.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318776B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-a6e60a1341bb4268aa4e7d1b1884a842 |
| Source note | uspto-grants-2012_11 |