참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Lithium Hydroxide | HCID 3939 | — |
| 반응물 | Ethyl bromoacetate | HCID 7748 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | HCID 67358777 | HCID 67358777 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(2-Oxo-3-(4-(trifluoromethyl)phenyl)pyrrolidin-1-yl)acetic acid | HCID 67358165 | — |
반응 단계
To a solution of the product from Example 266C (3.1 g, 13.00 mmol) in tetrahydrofuran (40 mL) was added potassium tert-butoxide (1.0 Min tetrahydrofuran, 15.7 mL, 15.7 mmol) via syringe under nitrogen, and the resultant mixture was stirred for 15 minutes. Then ethyl 2-bromoacetate (1.59 mL, 14.4 mmol) was added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated and then diluted with ethyl acetate, washed with water and brine, dried over magnesium sulfate, filtered and concentrated. The resulting residue was dissolved in ethanol/water (4:1, 60 mL) and treated with lithium hydroxide (1.254 g, 52.4 mmol). After stirring for 2 hours at reflux, the reaction was concentrated, diluted with ice/water (150 mL) and neutralized with 2 N HCl. The precipitate formed was filtered, washed with water (50 mL), and dried under vacuum to obtain the title compound. MS (DCI+) m/z 288.1 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08044069B2 |
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| 출처 데이터셋 | uspto-grants-2011_10 |
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| ORD ID | ord-19d6584a1a644160b683ab284742f40b |
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| 출처 메모 | uspto-grants-2011_10 |
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