関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 6-Bromohexanoic acid | HCID 20210 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3,4-Dichloro-2-propylphenol | HCID 600360 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Hexamethylphosphoramide | HCID 12679 | — |
| 生成物 | 6-(2-Propyl-3,4-dichlorophenoxy)hexanoic acid | HCID 14233046 | — |
反応手順
To a solution of 1.1 g. of 2-propyl-3,4-dichlorophenol in 30 ml. of tetrahydrofuran and 30 ml. of hexamethylphosphoramide were added 4.1 g. of 6bromohexanoic acid. To the solution were then added 1.3 g. of a 50% oil dispersion of sodium hydride. A catalytic amount of potassium iodide was added and the reaction was stirred under a nitrogen atmosphere at 60°-70° C. overnight. The reaction was cooled to room temperature and ethyl acetate and water were added. The solution was evaporated to dryness. Fresh ethyl acetate and water were added and the layers were separated. Fresh ethyl acetate was added to the aqueous layer and the aqueous layer was adjusted to pH 2. The layers were separated and the organic layer was washed with a saturated sodium chloride solution. The organic layer was then filtered through sodium sulfate and evaporated to dryness. The resulting residue was extracted with hexane and evaporated to dryness to afford 500 mg. of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04764521 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-e251a63eb2424cdea2c6965031dc78a9 |
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| 出典メモ | uspto-grants-1988_08 |
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