HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → N-(4,4-dimethylcyclohexylidene)hydroxylamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Cyclohexanone, 4,4-dimethyl- | HCID 138166 | — |
| Edukt | Hydroxyamine hydrochloride | HCID 443297 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | N-(4,4-dimethylcyclohexylidene)hydroxylamine | HCID 279448 | 80,4% |
Reaktionsschritte
To 4,4-Dimethylcyclohexanone (50 g, 396.19 mmol), NH2OH.HCl (35.84 g, 515.75 mmol) in H2O (190 mL) and ethanol (250 mL) was added a solution of Na2CO3 (54.16 g, 510.99 mmol) in water (170 mL) dropwise over a period of 20 minutes. After complete addition, reaction mixture was heated to reflux for 3h. The ethanol was evaporated, and the residue extracted into ethyl acetate (4×120 mL). The combined organic layer was washed with water (150 mL), brine (150 mL) and dried over sodium sulfate and concentrated to afford 45 g (80.4%) 4,4-dimethyl cyclohexanone oxime (I 6a) as white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09447039B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-e03278eef4564eb4a7b51ecd215cd9c5 |
| Quellennotiz | uspto-grants-2016_09 |