関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Amino-4-chlorophenol | HCID 7265 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,5-Dichlorobenzoyl chloride | HCID 76191 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(5-Chloro-2-hydroxyphenyl)-3,5-dichlorobenzamide | HCID 17860185 | 32.4% |
反応手順
2-Amino-4-chlorophenol (316 mg, 2.2 mmol) and triethylamine (243 mg, 2.4 mmol) were dissolved in dichloromethane (5 mL). A solution of 3,5-dichlorobenzoyl chloride (419 mg, 2 mmol) in dichloromethane (2 mL) was added dropwise under ice cooling and argon atmosphere, and the mixture was stirred at room temperature for 15 hours. After the reaction mixture was diluted with ethyl acetate, washed with water and brine one after another, dried over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (n-hexane-ethyl acetate=3:1) to give a light brown solid. The solid was suspended and washed with n-hexane-ethyl acetate under heating at reflux to give the title compound (205 mg, 32.4%) as a white crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08097759B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-06a72b8dc54d40c29f944b16309e5c38 |
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| 出典メモ | uspto-grants-2012_01 |
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