Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | 3,5-Dichlorobenzonitrile | HCID 81052 | — |
| Edukt | Magnesium | HCID 5462224 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3',5'-Dichloroacetophenone | HCID 2758058 | — |
Reaktionsschritte
A solution of methyl iodide (4 mL) in anhydrous Et2O (40 mL) was dropped into a suspension of magnesium (1.6 g) in anhydrous Et2O (16 mL) under a Nitrogen atmosphere. At the end of the dropping, benzene (120 mL) was added and the Et2O eliminated with a Nitrogen flux. Then, a solution of 3,5-dichlorobenzonitrile (4 g) in benzene (48 mL) was added and the mixture was heated to reflux for 3 hours. The solution was cooled to 0° C. and a 6N hydrochloric acid solution was added and the mixture was stirred overnight at r.t. Water and Et2O were added and the layers were separated. The organic phase was washed with a saturated sodium hydrogen carbonate solution and brine, dried and concentrated in vacuo. The residue was purified by flash chromatography (CH/AcOEt 95:5) to give the title compound (2.55 g) as an orange oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07214680B2 |
|---|
| Quelldatensatz | uspto-grants-2007_05 |
|---|
| ORD ID | ord-6242f81b8dbc4a129f3e525f0c94c963 |
|---|
| Quellennotiz | uspto-grants-2007_05 |
|---|