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Hydrochloric Acid → 4-Fluorohippuric acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | 4-Fluorobenzoyl chloride | HCID 67879 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 4-Fluorohippuric acid | HCID 699341 | 78.1% |
反応手順
A solution of glycine (15 g, 0.2 mol) in 175 mL of 5% aqueous sodium hydroxide is cooled to 10° C. to 15° C. p-Fluorobenzoyl chloride (31.6 g, 0.2 mol) is then added dropwise to the mixture and stirred vigorously for 0.5 hour while maintaining the temperature of the mixture of about 10° C. to 15° C. The pH of the reaction mixture is maintained at pH>9 by the dropwise addition of 50% aqueous sodium hydroxide. The mixture is stirred at 10° C. to 15° C. for two hours and the resulting clear solution then acidified to pH-1 with concentrated HCl. The resulting product is filtered off, washed with water (2×100 mL) and air dried to give a white solid (30.8 g, 78.1%); mp=161°-163° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727155 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-cd9cee84bbb34d60b58548e31996ec0e |
| 出典メモ | uspto-grants-1988_02 |