HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 86745179, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 15008262 | HCID 15008262 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 86745179 | HCID 86745179 | 78.3% |
Reaction Steps
A solution of (4-amino-3-pyridinyl)cyclohexylmethanone (5 g) and hydroxylamine hydrochloride (10 g) in 70 ml pyridine was stirred at 80° C. for three hours and thereafter concentrated. The residue was stirred with water, basified with sodium carbonate and extracted with dichloromethane. The organic extract was washed with water and saturated sodium chloride solution. The dried (anhy. MgSO4) organic layer was concentrated to 9 g waxy solid. This solid was triturated with acetonitrile to yield 4.9 g solid, m.p. 155°-158° C. Three grams were converted to the hydrochloride salt in methanol/ether to yield 2.8 g solid, m.p. 226°-228° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05095019 |
| Source dataset | uspto-grants-1992_03 |
| ORD ID | ord-0b92833604514f5da01fd00047ea4955 |
| Source note | uspto-grants-1992_03 |