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5-Bromo-1,2,3-trimethoxybenzene → HCID 178418846、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Bromo-1,2,3-trimethoxybenzene | HCID 75885 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 178418846 | HCID 178418846 | — |
反応手順
To a stirred solution of n-butyllithium (3.7 mL, 1.6 M in hexane solution,6.0 mol) in dry ether (40 mL), a solution of 3,4,5-trimethoxyphenylbromide (0.74 g, 3.0 mol) in ether (20 mL) was added under dry nitrogen at −78° C. The solution was stirred for 1 h in order to form 3,4,5-trimethoxyphenyllithum (“TPL”). Substituted tetralone reagent (3.0 mol) was added at −20° C., and the stirring was continued for 2 h (−20° C.-RT). The mixture was partitioned between CH2Cl2 and water, the organic layer was dried over anhydrous sodium sulfate, and, after filtration, the organic layer was concentrated in vacuo to provide a tetrahydronaphthalen-1-ol as a yellow oil. Each compound was purified by column chromatography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091240B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-44b54a3e212a410d8860722b1d5535c3 |
| 出典メモ | uspto-grants-2006_08 |