HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl Sulfate → 3,6-Dimethoxyphthalonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl Sulfate | HCID 6497 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2,3-Dicyanohydroquinone | HCID 78467 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | 3,6-Dimethoxyphthalonitrile | HCID 358358 | — |
Reaktionsschritte
Dimethyl sulfate (15 mL, 0.16 mol) and anhydrous potassium carbonate (24 g, 0.17 mol) are added to a solution of 2,3-dicyanohydroquinone (3.0 g, 0.019 mol) in 100 mL 2-butanone. The reaction mixture is refluxed for 18 hr. under a stream of argon, cooled to room temperature and the resulting solid is collected by filtration. The residue is added to water (100 mL) to dissolve the potassium carbonate and the resulting insoluble material is collected by filtration and dried under vacuum to yield 3.10 g (88%), m.p. 276°-280° C., 1H NMR (DMSO-d6) in ppm, δ=7.63 (s, 2H), 3.93 (s, 6H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05679661 |
| Quelldatensatz | uspto-grants-1997_10 |
| ORD ID | ord-0d1805e881f04a3392b2c13022f9e162 |
| Quellennotiz | uspto-grants-1997_10 |