関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Isoquinoline-5-carboxaldehyde | HCID 7016853 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-(Isoquinolin-5-yl)ethanol | HCID 20493434 | 97% |
反応手順
To a mixture of Mg turnings (0.2 g, 7.9 mmol) in ether (10 mL) was added MeI (1.13 g, 7.9 mmol) slowly at RT under an inert atmosphere. After being stirred for 1 h at RT, the reaction mixture was cooled to −10° C. and a solution of isoquinoline-5-carbaldehyde (0.5 g, 3.18 mmol) in ether (10 mL) was added. The reaction mixture was then stirred for an additional hour at RT, quenched with saturated NH4Cl solution and extracted with EtOAc (3×50 mL). The combined organic layers were washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo to obtain the crude product. The crude material was purified via silica gel column chromatography using 30% ethyl acetate in hexanes to afford 1-(isoquinolin-5-yl)ethanol (0.53 g, 97%) as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481532B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-7ac68687a3e74ebbb9e91eb9a2001f71 |
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| 出典メモ | uspto-grants-2013_07 |
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