関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (3-(Methylsulfonyl)propyl 4-methylbenzenesulfonate | HCID 22732325 | — |
| 反応物 | [4-Hydroxy-3'-(hydroxymethyl)-6-methylbiphenyl-2-yl]methyl acetate | HCID 59342611 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (3'-(Hydroxymethyl)-6-methyl-4-[3-(methylsulfonyl)propoxy]biphenyl-2-yl)methyl acetate | HCID 59342573 | 60.1% |
反応手順
To a solution of [4-hydroxy-3′-(hydroxymethyl)-6-methylbiphenyl-2-yl]methyl acetate (1.02 g, 3.56 mmol) and 3-(methylsulfonyl)propyl 4-methylbenzenesulfonate (1.25 g, 4.27 mmol) in N,N-dimethylformamide (10 mL) was added potassium carbonate (0.640 g, 4.32 mmol), and the mixture was stirred at 90° C. for 21 hr under nitrogen atmosphere. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=50:50-100:0) to give the title compound (0.87 g, yield 60%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08492430B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-f95f4c9b1f364c72bb633aae5e141901 |
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| 出典メモ | uspto-grants-2013_07 |
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