関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4,6-Trichlorophenol | HCID 6914 | — |
| 反応物 | Benzylmalonic acid | HCID 12031 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | Bis(2,4,6-trichlorophenyl) benzylpropanedioate | HCID 2782299 | — |
反応手順
A mixture of 2-benzylmalonic acid (10.0 g, 51.5 mmol), 2,4,6-trichlorophenol (20.3 g, 103 mmol), and POCl3 (12.0 mL, 129 mmol) was stirred under air at 105° C. for 2 hours. The reaction was then cooled to room temperature, poured on 150 mL ice, and extracted with 4:1 ether/DCM (3×150 mL). The combined organic layers were washed with water (1×400 mL) and 4 M aqueous NaCl (1×100 mL), and the yellow organic layer was dried (Na2SO4), filtered, and concentrated by rotary evaporation at <40° C. to provide the title compound as a tan thick oil that became a beige solid upon standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09290476B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-65d5e616cc48453390f5f22d30d5e56a |
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| 出典メモ | uspto-grants-2016_03 |
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