関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Fluorophenylhydrazine hydrochloride | HCID 2723914 | — |
| 反応物 | 7-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one | HCID 13011007 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | HCID 66834755 | HCID 66834755 | 50% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440922B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-ba7e0ff52b4e47e9bdf6c40c89c10e9b |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|
