関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 2-(bromomethyl)benzoate | HCID 2734813 | — |
| 反応物 | N-benzyl-N-hexyl-3-(4-hydroxyphenyl)propanamide | HCID 69120664 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 2-[(4-{3-[benzyl(hexyl)amino]-3-oxopropyl}phenoxy)methyl]benzoate | HCID 69120482 | 34.6% |
反応手順
N-benzyl-N-hexyl-3-(4-hydroxyphenyl)propanamide (183 mg, 0.54 mmol), methyl 2-(bromomethyl)benzoate (136 mg, 0.59 mmol) and potassium carbonate (112 mg, 0.81 mmol) were mixed in acetonitrile. The mixture was stirred at 66° C. overnight. The solvent was evaporated under reduced pressure and the residue was dissolved in ethyl acetate. The organic phase was washed (water ×2, brine ×1), dried (Na2SO4) and evaporated. Further purification by preparative HPLC (using a gradient of CH3CN/10% CH3CN-waterphase containing 0.1M NH4OAc as eluant) gave 91 mg (yield 34%) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07355069B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-b30401a69e314a9f874f0f8afe1d5d46 |
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| 出典メモ | uspto-grants-2008_04 |
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