HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethylene Glycol → (1E)-1-methoxyimino-1-(2-methyl-1,3-dioxolan-2-yl)propan-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethylene Glycol | HCID 174 | — |
| Edukt | Trimethyl orthoformate | HCID 9005 | — |
| Edukt | Diacetyl(methoxyimino)methane | HCID 536122 | — |
| Katalysator | p-Toluenesulfonic acid | HCID 6101 | — |
| Produkt | (1E)-1-methoxyimino-1-(2-methyl-1,3-dioxolan-2-yl)propan-2-one | HCID 22967234 | 79,4% |
Reaktionsbedingungen
| Temperatur | 85 °C |
|---|
Reaktionsschritte
2400 g (39 mol) of ethylene glycol, 430 g (3.62 mol) of trimethyl orthoformate, 550 g (3.9 mol) of pentane-2,3,4-trione 3-(O-methyloxime) and 9 g of p-toluene sulfonic acid (46 mmol) were heated with stirring to 85° C. over a period of 15 min. After 30 min at 85° C., the mixture was cooled to room temperature. During the reaction, volatile components were distilled off via a column head. For work-up, the mixture was washed with saturated sodium bicarbonate solution and extracted with methyl tert-butyl ether, and the combined organic phases were washed twice with water and finally dried over magnesium sulfate. Distillative removal of the solvent gave 580 g of a red-brown oil (phys. data see Tab. 1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06441236B1 |
| Quelldatensatz | uspto-grants-2002_08 |
| ORD ID | ord-c53fe3edc8674c529c8e128872e6fe7a |
| Quellennotiz | uspto-grants-2002_08 |