HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 3-Chloro-2-methyl-6-nitrobenzonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | 2,6-Dichloro-3-nitrotoluene | HCID 97155 | — |
| Edukt | HCID 178418546 | HCID 178418546 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 3-Chloro-2-methyl-6-nitrobenzonitrile | HCID 22008961 | 60,2% |
Reaktionsschritte
A solution of 10 g (49 mmol) of 2,6-dichloro-3-nitrotoluene and 4.8 g (54.0 mmol) of CuCN in 100 ml of abs. DMF was stirred at 150° C. for 6 h, a further 2.4 g (27.0 mmol) of CuCN being added after 4 h. The solvent was stripped off and the residue obtained taken up in ethyl acetate. The precipitate deposited was filtered off and extracted several times with warm ethyl acetate. The combined ethyl acetate solutions were washed with H2O, dilute ammonia solution, and saturated NaCl solution, dried over Na2SO4, and concentrated to dryness. The resulting yellow, crystalline residue was purified by column chromatography on SiO2 using EA/n-heptane 1:10 as a solvent. 5.8 g of the title compound resulted in the form of yellow crystals.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06211196B1 |
| Quelldatensatz | uspto-grants-2001_04 |
| ORD ID | ord-dee4e1ef582640dcb0215f4430dde985 |
| Quellennotiz | uspto-grants-2001_04 |