関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Hydrazinopyridine | HCID 78645 | — |
| 反応物 | 7-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one | HCID 13011007 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 8-Methoxy-10,10-dimethyl-10,11-dihydro-5H-1,11-diaza-benzo[B]fluorene | HCID 66833905 | — |
反応手順
2-Hydrazinopyridine (1.3 g, 11.8 mmol) and 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 2.4 g, 11.8 mmol) were dissolved in NMP (60 mL), and stirred at 190° C. for 48 hr. The reaction solution was diluted with ethyl acetate, washed with water and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the target compound (white solid, 101 mg, 3%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440922B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-d2cfd862385d4e1bbadc5347e9025ed2 |
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| 出典メモ | uspto-grants-2016_09 |
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