関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 4-[[3,5-bis(trimethylsilyl)benzoyl]amino]-2-fluorocinnamate | HCID 68484203 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-[[3,5-Bis(trimethylsilyl)benzoyl]amino]-2-fluorocinnamic acid | HCID 68482121 | 55% |
反応手順
Compound 2b (80 mg) was dissolved in ethanol (2.6 ml), and a 2N sodium hydroxide aqueous solution (1.7 ml) was added to the obtained solution in a nitrogen atmosphere. The mixture was stirred overnight at room temperature. A 2N hydrochloric acid aqueous solution (3.4 ml) was added thereto. The resulting white precipitate was filtered off and dissolved in ethyl acetate. The reaction mixture was separated with ethyl acetate and water. The organic layer was washed with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. After the solvent was distilled off and n-hexane was added to the obtained residue, the mixture was pulverized with ultrasonic waves. The solid was filtered off, and the obtained powder was dissolved in butyl acetate (0.5 ml) by heating. The reaction mixture was allowed to cool and then filtered. Thus, Compound 2 (39 mg, 55%) was obtained as an opalescent solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07855300B2 |
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| 出典データセット | uspto-grants-2010_12 |
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| ORD ID | ord-46a0dffe7def4a2c8d0d8766d6f42794 |
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| 出典メモ | uspto-grants-2010_12 |
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