関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylparaben | HCID 8434 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Butanol, 4-chloro-, 1-acetate | HCID 23399 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Hydroxybutoxy)benzoic acid | HCID 15218596 | 89.5% |
反応手順
276.6 g of 4-chlorobutyl acetate (1.8 mol) were added to a solution of 249 g of ethyl 4-hydroxybenzoate (1.5 mol), 3 g of potassium iodide (0.018 mol) and 248 g of potassium carbonate (1.8 mol) in 21 of DMF, and the mixture was stirred at 90° C. for 11 hours. The reaction mixture was poured into 5 l of ice-water, and the precipitate was filtered off with suction and washed with 41 of ice-water. The crude product was dissolved in 3 l of ethanol, potassium hydroxide (400 g) was added, and the mixture was refluxed for 3 hours. The reaction mixture was poured into 6 l of ice-water and acidified using concentrated hydrochloric acid, and the precipitate was filtered off. The precipitate was washed with water until neutral and subsequently dried, giving 282.1 g of 4-(4′-hydroxybutoxy)benzoic acid (yield 89%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06486338B1 |
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| 出典データセット | uspto-grants-2002_11 |
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| ORD ID | ord-997e80863f7e40ffab1855ebc2c7920c |
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| 出典メモ | uspto-grants-2002_11 |
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