HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → HCID 178481735, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Dimethyl Sulfate | HCID 6497 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | HCID 178515597 | HCID 178515597 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | HCID 178481735 | HCID 178481735 | 67,2% |
Reaktionsschritte
30 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1H-pyrazole from Example 3.1 were initially charged in 750 ml of toluene. 23.1 g of dimethyl sulfate and 7.5 g of potassium carbonate were added, and the mixture was heated at reflux for 2 h. After cooling to room temperature, the mixture was made alkaline using ammonia and stirred overnight. The mixture was acidified by addition of hydrochloric acid (pH about 1) and cooled to room temperature, and the precipitated solid was filtered off. Drying gave 21.4 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1-methyl-1H-pyrazole (purity according to GC 99.2%, yield 66.8%). M.p.: 128° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06897322B2 |
| Quelldatensatz | uspto-grants-2005_05 |
| ORD ID | ord-7699cd7ee4c345c598cec46a2ba68854 |
| Quellennotiz | uspto-grants-2005_05 |