関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4,4-Dimethyl-3,4-dihydro-2H-naphthalen-1-one | HCID 236547 | — |
| 反応物 | HCID 178418306 | HCID 178418306 | — |
| 生成物 | 3,4-Dihydro-4,4-dimethyl-6-acetyl-1-(1,1-dimethlethyl)naphthalene | HCID 22571553 | — |
反応手順
To a solution of 6-(2-methyl-1,3-dioxolan-2-yl)!-3,4-dihydro-4,4-dimethylnaphthlen-1(2H)-one ((Compound D15, 353 mg, 1.36 mmol) in 3 ml of dry ether at -78° C. was added dropwise t-BuLi (1 ml, 1.7 mmol, 1.7M solution in pentane). This dear light yellow solution was left at -78° C. for 30 min. Then, fleshly distilled SOCl2 (0.15 ml, 2.0 mmol) was added. The reaction mixture was stirred at -78° C. for additional 30 min and thereafter slowly warmed to room temperature. The reaction was quenched by addition of saturated NH4Cl. The white solids were removed by filtration and the clear solution was concentrated to an oil, and purified by column chromatography with ethyl acetate/hexane (1/10) to give the title compound as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05723666 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-130b3a00a9dc43f5a473799157e45ada |
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| 出典メモ | uspto-grants-1998_03 |
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