HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Calcium Fluoride → Methyl 4-(fluoromethyl)benzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Calcium Fluoride | HCID 84512 | — |
| Edukt | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| Edukt | Potassium Fluoride | HCID 522689 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Methyl 4-(fluoromethyl)benzoate | HCID 21866613 | 78,7% |
Reaktionsschritte
Dry acetonitrile (150 ml) was added to 25.00 g of methyl 4-(bromomethyl)benzoate, 19.02 g of potassium fluoride and 9.51 g of calcium fluoride, and the mixture was heated to reflux for 3 days. The reaction solution was concentrated. After addition of 200 ml of acetonitrile, insolubles were removed by filtration, and the filtrate was concentrated again. The residue was purified by silica gel column chromatography (YMC•GEL® SIL-60-230/70, n-hexane:ethyl acetate=10:1–4:1), followed by distillation under reduced pressure to provide 14.45 g of the objective compound as colorless oil. B.p. 118.5–119° C./18 mmHg.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06998412B2 |
| Quelldatensatz | uspto-grants-2006_02 |
| ORD ID | ord-da8c24c5b365428ca729435422979881 |
| Quellennotiz | uspto-grants-2006_02 |