HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 86752926, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-Chloro-5-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]benzaldehyde | HCID 18692932 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86752926 | HCID 86752926 | — |
Reaction Steps
22.6 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine, 6.5 g of sodium bicarbonate and 5.4 g of hydroxylamine hydrochloride in 100 ml of tetrahydrofuran were stirred at 23° C. for 24 hours. The tetrahydrofuran was then removed, after which the residue was taken up in 100 ml of methylene chloride. The solution was washed twice with 100 ml of water. The solid formed during this was removed, washed with water and dried. Concentration of the organic phase resulted in a residue which was purified by chromatography on silica gel with cyclohexane/ethyl acetate (7:3). Yield: 26.1 g (82%) of colorless crystals; melting point: 173°-174° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05783522 |
| Source dataset | uspto-grants-1998_07 |
| ORD ID | ord-5ab8592f646b46b2be451895b282f07a |
| Source note | uspto-grants-1998_07 |