HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Pyridine → 4-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Thionyl Chloride | HCID 24386 | — |
| Edukt | 4-methyl-N-(2,2,2-trichloro-1-hydroxyethyl)benzamide | HCID 3392664 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide | HCID 12341576 | 89,2% |
Reaktionsschritte
A stirred solution of Example 37C (20.0 g, 70.8 mmol) in CH2Cl2(300 mL) at 0° C. was treated with pyridine (10 mL). The reaction mixture was treated dropwise with thionyl chloride (10.4 mL, 141 mmol), and the reaction flask was equipped with a calcium chloride drying tube. The reaction mixture was warmed to ambient temperature and stirred for 4 hours. Concentration of the reaction mixture to a reduced volume and addition of diethyl ether (100 mL) resulted in a precipitate which was filtered off, and the filtrate was concentrated and dried under reduced pressure to provide 19.0 g of the desired product as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06645968B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-3714a12322254811b07426d335532996 |
| Quellennotiz | uspto-grants-2003_11 |