HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → [(4-Chloro-1H-pyrazol-1-yl)oxy]methyl thiocyanate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Thiocyanic acid, chloromethyl ester | HCID 76755 | — |
| Edukt | Tetrabutylammonium Hydroxide | HCID 2723671 | — |
| Edukt | 4-Chloro-1H-pyrazol-1-ol | HCID 13391252 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | [(4-Chloro-1H-pyrazol-1-yl)oxy]methyl thiocyanate | HCID 14011041 | 71,6% |
Reaktionsschritte
50 ml of a 5% strength aqueous sodium hydroxide solution were added to 5 g (42 mMol) of 4-chloro-1-hydroxypyrazole, 13.5 g (126 mMol) of chloromethyl thiocyanate and 50 ml of methylene chloride. After the addition of 1 g (4 mMol) of tetra-n-butylammonium hydroxide, the mixture was stirred at room temperature for 24 hours. Thereafter, the organic phase was separated off, dried and evaporated down. Distillation of the residue under reduced pressure (airbath at 140° C./3 mbar) gave 5.7 g (71% of theory) of 4-chloro-1-[(thiocyanato)-methoxy]-pyrazole (compound No. 1), which was recrystallized from ether/petroleum ether (mp. 60° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04764527 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-e1f2e11ee6ab46f19657e1637b95bd26 |
| Quellennotiz | uspto-grants-1988_08 |