関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | 1,3-Dibromopropane | HCID 8001 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Methyl alpha-methylbenzeneacetate | HCID 569653 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 5-bromo-2-methyl-2-phenyl-pentanecarboxylate | HCID 22995606 | — |
反応手順
15 g (0.234 mol) of n-butyl lithium as a 2.5 molar solution in hexane are added dropwise to a solution of 32.8 ml (0.234 mol) of diisopropylamine in 200 ml of anhydrous tetrahydrofuran at −30° C. and stirred for 10 minutes at −10° C. 38.4 g (0.234 mol) of methyl 2-phenylpropionate are added dropwise at −76° C. and stirred for 30 minutes at this temperature. Then 26.3 ml (0.257 mol) of 1,3-dibromopropane are added, when the addition has ended the cooling bath is removed and the mixture is stirred for 14 hours at ambient temperature. The reaction solution is poured onto 1.2 l of water and extracted with diethylether. The organic phases are extracted with water, dried over sodium sulphate and the solvent is removed. The residue is distilled under high vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06617325B1 |
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| 出典データセット | uspto-grants-2003_09 |
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| ORD ID | ord-17cecb85e5184900a32903ea401b91a3 |
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| 出典メモ | uspto-grants-2003_09 |
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