関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 5-Methoxy-2-methyl-2-(3-oxo-butyl)-1-indanone | HCID 21990908 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-methoxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one | HCID 21990903 | 99.1% |
反応手順
Pyrrolidine (0.159 mL, 1.9 mmol) and acetic acid (0.109 mL, 1.9 mmol) were added to a solution of 5-methoxy-2-methyl-2-(3-oxo-butyl)-1-indanone (467 mg, 1.9 mmol) in toluene (5 mL) and the resulting solution was heated in an oil bath at 85° C. for 2.5 hours. After cooling to room temperature, the reaction mixture was diluted with EtOAc (20 mL), washed with water (20 mL), 5% NaHCO3 (20 mL), and brine (10 mL), dried over MgSO4, filtered, and evaporated under vacuum to yield 7-methoxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (430 mg) as a light brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087599B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-d6636cf7073446fb80a814617775f2cf |
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| 出典メモ | uspto-grants-2006_08 |
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