참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 4-(4-Oxo-4-phenyl-butyryl)-benzoic acid ethyl ester | HCID 4452032 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(4-Oxo-4-phenyl-butyryl)-benzoic acid | HCID 57423666 | 99.8% |
반응 단계
4-(4-Oxo-4-phenyl-butyryl)-benzoic acid ethyl ester (3.22 g, 10.4 mmol) is dissolved in THF (100 mL) and an aqueous solution of KOH (15.6 mmol in 50 mL) is added. The reaction is stirred and heated (65° C.) for 6 h, whereupon HPLC analysis indicated the formation of a single product at the expense of the diketone. The reaction is neutralized with aqueous HCl and the THF removed in vacuo. The resulting solid is dissolved in EtOAc and the organic phase dried (Na2SO4), filtered and concentrated to afford 2.93 g (>99%) of the desired carboxylic acid (RT=0.90). LCMS confirmed the identity of the product (ES+Exact Mass: 282.09, Obs.: 283.48). This product is used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07488832B2 |
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| 출처 데이터셋 | uspto-grants-2009_02 |
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| ORD ID | ord-1e6484ba8d164384850040eca40f606d |
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| 출처 메모 | uspto-grants-2009_02 |
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