関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Monomethyl terephthalate | HCID 15513 | — |
| 反応物 | 2-Amino-4'-methoxyacetophenone hydrochloride | HCID 12487188 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-(4-Methoxycarbonylbenzamido)-4'-methoxyacetophenone | HCID 13640369 | 92.1% |
反応手順
To a solution of 2-amino-4′-methoxyacetophenone hydrochloride (5.33 g) in pyridine (4.28 ml), triethylamine (3.68 ml) and dichloromethane (50 ml) was added dropwise a solution of terephthalic acid monomethyl ester (5.25 g) in dichloromethane (10 ml) at 0° C. The reaction mixture was allowed to warm to room temperature, and stirred for 3 hours. To the reaction mixture was added dichloromethane (200 ml), washed with 1N-sodium hydroxide (100 ml×2), saturated hydrogen carbonate aqueous solution (100 ml×2) and brine, and dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure. The solids were slurried in n-hexane, and collected by filtration to give 2-(4-methoxycarbonyl-benzamido)-4′-methoxyacetophenone (7.97 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06331521B1 |
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| 出典データセット | uspto-grants-2001_12 |
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| ORD ID | ord-6166f9853aa6469cbc73aef21e32c70a |
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| 出典メモ | uspto-grants-2001_12 |
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