HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-methylhydroxylamine hydrochloride → Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Edukt | ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate | HCID 53690408 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate | HCID 15070019 | — |
Reaktionsschritte
18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0.108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05416096 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-c363c3f6a8394ce3b9913ed620fe0370 |
| Quellennotiz | uspto-grants-1995_05 |