참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Pyrrolidine | HCID 31268 | — |
| 반응물 | 3-[(2-Acetylthiomethyl-3-phenylpropionyl)amino]-5-ethylbenzoic acid | HCID 15670211 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-[(2-Mercaptomethyl-3-phenylpropionyl)amino]-5-ethylbenzoic acid | HCID 15670212 | 33.7% |
반응 단계
3-[(2-Acetylthiomethyl-3-phenylpropionyl)amino]-5-ethylbenzoic acid (compound of Example 64) (1.0 g) is suspended in water (10 ml), and thereto is added pyrrolidine (0.6 g) under nitrogen, and the mixture is stirred at room temperature for 20 minutes. The reaction mixture is adjusted to pH 1 with conc. hydrochloric acid and is extracted with ethyl acetate (100 ml). The extract is washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and ethyl acetate is distilled off under reduced pressure. The residue is dissolved in methanol and purified by a medium pressure column chromatography with CHP-20P (eluant, water-methanol). The fractions containing the desired compound are collected and concentrated into dryness to give the title compound (0.3 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05210266 |
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| 출처 데이터셋 | uspto-grants-1993_05 |
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| ORD ID | ord-92c2d479c2fb462a936f028f5a28c2dd |
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| 출처 메모 | uspto-grants-1993_05 |
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