참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (2S,3R)-methyl-2-benzamidomethyl-3-hydroxybutyrate | HCID 10060699 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 생성물 | HCID 10975521 | HCID 10975521 | 80% |
반응 단계
20.08 g (0.08 mole) of methyl (2S,3R)-2-(N-benzoyl amino)methyl-3-hydroxybutyrate were dissolved in 60.8 g of 12N-hydrochloric acid solution, refluxed with application of heat for 6 hours and cooled to room temperature, so that a solid was precipitated. After the solid was filtered, the filtrate was washed twice with 100 ml of toluene. Then a water phase was concentrated to a residue in vacuo. To this was added 250 ml of acetonitrile and further, under an ice water cooling, 0.08 g (0.08 mole) of triethylamine. The total solution was stirred overnight at room temperature to yield precipitates. The precipitates were filtered, washed with 200 ml of acetonitrile and dried in vacuo, thereby obtaining 8.51 g (0.06 mole) of (2S,3R)-2-aminomethyl-3-hydroxybutyric acid. Yield was 80%. This compound corresponded to that described in the Japanese published application Hei 2-134 349 according to an 1H-NMR spectrum analysis.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05712388 |
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| 출처 데이터셋 | uspto-grants-1998_01 |
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| ORD ID | ord-04573850af834060bea86b2fadf1c5b5 |
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| 출처 메모 | uspto-grants-1998_01 |
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