HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Ethyl 3-chlorobenzyl[2,4-dinitro-6-(trifluoromethyl)phenyl]carbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)- | HCID 67851 | — |
| Edukt | Ethyl [(3-chlorophenyl)methyl]carbamate | HCID 17071127 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Ethyl 3-chlorobenzyl[2,4-dinitro-6-(trifluoromethyl)phenyl]carbamate | HCID 20827739 | 9,4% |
Reaktionsschritte
Ethyl 3-chlorobenzylcarbamate (720.3 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (829.1 mg) were dissolved in tetrahydrofuran (20 ml), and to the solution was added sodium hydride (147.1 mg). The reaction mixture was heated at reflux for 1.5 hours. After allowing to cool, to the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=10:1) to give the title compound (129.5 mg, 9%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06939887B2 |
| Quelldatensatz | uspto-grants-2005_09 |
| ORD ID | ord-65ef8bcd7f7e4b638673690370d62ffb |
| Quellennotiz | uspto-grants-2005_09 |