HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trimethyl orthoformate → 1-(1,1-Dimethoxyethyl)-2,4-difluorobenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trimethyl orthoformate | HCID 9005 | — |
| Edukt | 2,4-Difluoroacetophenone | HCID 67770 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Katalysator | p-Toluenesulfonic acid | HCID 6101 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 1-(1,1-Dimethoxyethyl)-2,4-difluorobenzene | HCID 57752280 | — |
Reaktionsschritte
In a solution composed of 15.7 g of 2,4-difluoroacetophenone, 35 g of trimethyl ortho-formate and 15 g of methanol, 0.96g of p-toluenesulfonic acid was added, and reacted at 40° C. to 45° C. for 2 hours. This was added to an aqueous solution of 5% by mass sodium hydrogen carbonate, which was then extracted with ethyl acetate. An extract was washed with water, and dried on Na2SO4. Then, ethyl acetate was concentrated to yield 18.2 g of 1-(1,1-dimethoxyethyl)-2,4-difluorobenzene. It was confirmed that the 1-(1,1-dimethoxyethyl)-2,4-difluorobenzene had NMR data of (CDCl3, δppm) 1.62 (s, 3H), 3.9 (s, 6H), 6.74-6.9 (m, 2H), 7.56-7.7 (m, 1H) by NMR (supplied from Varian Technologies Japan Limited).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07556911B2 |
| Quelldatensatz | uspto-grants-2009_07 |
| ORD ID | ord-f5a86ba414ad4793a8b3bf01c1c1e5cc |
| Quellennotiz | uspto-grants-2009_07 |