HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Methyl [1-(2-((N,N-diphenylamino)carbamoyl)-1E-ethylidene)-1,2,3,4-tetrahydronaphthalen-5-yl]oxyacetate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Hydrazine, 1,1-diphenyl-, hydrochloride (1:1) | HCID 10738 | — |
| Edukt | Methyl [1-(2E-carboxyvinyl)-1,2,3,4-tetrahydronaphthalen-5-yl]oxyacetate | HCID 86750227 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Methyl [1-(2-((N,N-diphenylamino)carbamoyl)-1E-ethylidene)-1,2,3,4-tetrahydronaphthalen-5-yl]oxyacetate | HCID 86750228 | 70,8% |
Reaktionsschritte
A solution of the carboxylic acid (prepared in reference example 5, 150 mg), 2-chloro-N-methylpyridinum iodide (197 mg). 1,1-diphenylhydrazine hydrochloride (147 mg) and triethylamine (0.216 ml) in methylene chloride (6 ml) was stirred overnight at room temperature. The mixture was poured into 1N hydrochloric acid, and extracted with methylene chloride. The extract was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and evaporated. The residue was crystallized from crystallized ethyl acetate to give the title compound (as pale yellow powder; 167 mg) having the following physical data.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05596009 |
| Quelldatensatz | uspto-grants-1997_01 |
| ORD ID | ord-0ffa1781a30545b6a46a0fe793fac147 |
| Quellennotiz | uspto-grants-1997_01 |