関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Butyl-4-chloro-5-methoxy-2-(3-oxopentyl)-1-indanone | HCID 21990911 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 9a-butyl-8-chloro-7-methoxy-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one | HCID 21990876 | 60.6% |
反応手順
A solution of 2-butyl-4-chloro-5-methoxy-2-(3-oxo-pentyl)-1-indanone (250 mg, 0.74 mmol) in acetic acid (2 mL) was diluted with 6N aqueous HCl (2 mL). The resulting mixture was stirred and heated in an oil bath at 90° C. for 18 hours, then kept at room temperature for 2 days. The mixture was diluted with EtOAc (20 mL), washed with water (30 mL), 5% NaHCO3 (10 mL) and brine (5 mL), dried over MgSO4, filtered, and evaporated under vacuum to an oil (250 mg). The crude product was purified by preparative layer chromatography on three 0.1×20×20 silica gel GF plates, developing with 5% EtOAc in CH2Cl2, to afford 9a-butyl-8-chloro-7-methoxy-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (143 mg).
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-6121252028114c99b582eb81c90945f8 |
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| 出典メモ | uspto-grants-2006_08 |
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