HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 24754766, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 10862282 | HCID 10862282 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 24754766 | HCID 24754766 | 75% |
Reaction Steps
To a stirred suspension of hydroxylamine hydrochloride (2.74 g, 40 mmol) in dioxane (25 ml) sodium acetate (3.25 g, 40 mmol) in water (15 ml) was added dropwise at room temperature, followed by dropwise addition of 4-(5-p-methylphenyl-3-trifluoromethyl-pyrazol-1-yl)-benzenesulfonyl chloride (4.11 g, 10 mmol) in dioxane (40 ml). The obtained reaction mixture was poured into water (100 ml), extracted with ethyl acetate (2×50 ml), the organic layers were washed with water (3×50 ml) and brine (1×50 ml), dried over MgSO4, filtered and concentrated in vacuo. The obtained oil was crystallized from 75% aqueous ethanol (75 ml) to yield 2.94 g (75%) of the title compound as white crystals. Mp: 203° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07723370B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-30c47d4cd2d04af6bcf4ca56e95fb93c |
| Source note | uspto-grants-2010_05 |