Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | 3-Fluorophenylhydrazine hydrochloride | HCID 2723914 | — |
| Edukt | 7-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one | HCID 13011007 | — |
| Lösungsmittel | Ethyl acetate hexane | HCID 21226206 | — |
| Produkt | HCID 66834755 | HCID 66834755 | 50% |
Reaktionsschritte
Under nitrogen atmosphere, the acetic acid (1 mL) suspension of 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 101.0 mg, 0.495 mmol) and (3-fluoro-phenyl)-hydrazine hydrochloric acid salt (Compound V1, 96.5 mg, 0.593 mmol) was stirred at ambient temperature of 95° C. for 3.75 hr. After cooling to room temperature, the reaction mixture was added with water (1 mL) and hexane/ethyl acetate (15:1) (0.5 mL), and stirred at room temperature for 15 min. The solid was filtered, washed with hexane/ethyl acetate (15:1), and then dried under reduced pressure to obtain the title compound (beige powder, 72.7 mg, 50%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US09440922B2 |
|---|
| Quelldatensatz | uspto-grants-2016_09 |
|---|
| ORD ID | ord-ba7e0ff52b4e47e9bdf6c40c89c10e9b |
|---|
| Quellennotiz | uspto-grants-2016_09 |
|---|