関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chlorobenzenesulfonyl chloride | HCID 76187 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Benzyl 3-hydroxyphenyl ether | HCID 138048 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Methyl, chloro- | HCID 5378701 | — |
| 生成物 | 2-Chlorobenzenesulfonic acid 3-benzyloxyphenyl ester | HCID 54263647 | 95.2% |
反応手順
To a solution of 3-benzyloxyphenol (2.97 g, 15 mmol), as prepared in the preceding step, in methylene chlorine (50 mL) at 0° C., was added N,N-diisopropylethylamine (2 mL) and 2-chlorobenzenesulfonyl chloride (3.27 g, 15.5 mmol). The reaction mixture was stirred at 0° C. for 2 h and at room temperature for 2 h. The reaction mixture was diluted with methylene chloride (200 mL), washed sequentially with saturated NaHCO3 (2×50 mL) and brine (2×50 mL), dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography (1:1 hexane:methylene chloride) to give the title compound as a colorless liquid (5.35 g, 95%). 1H-NMR (300 MHz, CDCl3) δ 4.97 (s, 2H), 6.71 (dd, 1H), 6.78 (t, 1H), 6.85 (dd, 1H), 7.17 (t, 1H), 7.37 (m, 5H) 7.58 (m, 2H), 7.91 (dd, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05792769 |
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| 出典データセット | uspto-grants-1998_08 |
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| ORD ID | ord-5c3bcc26d948446b9669f45c51ee5114 |
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| 出典メモ | uspto-grants-1998_08 |
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