関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | HCID 178491344 | HCID 178491344 | — |
| 反応物 | HCID 178506846 | HCID 178506846 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Benzene--cyclohexane (1/1) | HCID 18624872 | — |
| 生成物 | HCID 178436445 | HCID 178436445 | — |
反応手順
To a solution of 10.0 g (38 mmol) [1-(2,6-dimethoxy-phenyl)-meth-(E)-ylidene]-(1-isopropyl-2-methyl-propyl)-amine in 30 ml dry THF cooled to −20° C. were added 91.2 ml of a 0.5M solution of ethyl lithium in cyclohexane/benzene drop-wise to keep temperature below 0° C. Then the mixture was stirred at −20° C. for further 30 min and the reaction quenched by addition of water. The aqueous phase was extracted with ethyl acetate, the combined extracts washed with brine, dried over Na2SO4, filtered and evaporated. Purification of the crude product by flash chromatography on silica gel with a heptane/ethyl acetate gradient provided 4.30 g (E)-[1-(2-ethyl-6-methoxy-phenyl)-methylidene]-(1-isopropyl-2-methyl-propyl)-amine as colourless liquid: MS (EI): 261.4 (M+.), 218.3 ((M-((CH3)2CH)+.), 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07875645B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-5f4e6ca46c3041f4a8d66df479d79769 |
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| 出典メモ | uspto-grants-2011_01 |
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