Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl chloroformate → N-(Methoxycarbonyl)-N-methyl-L-valine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl chloroformate | HCID 6586 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | N-Methyl-L-valine | HCID 444080 | — |
| 생성물 | N-(Methoxycarbonyl)-N-methyl-L-valine | HCID 59166373 | 71% |
반응 단계
(2S)-3-Methyl-2-methylamino-butanoic acid (5 g, 38.12 mmol) is added to a stirring solution of sodium hydroxide (76.2 mL of 1 M, 76.24 mmol). After complete dissolution, sodium carbonate (2.1 g, 19.82 mmol) is added followed by methyl chloroformate (3.18 mL, 41.17 mmol) at 0° C. over 40 minutes. The reaction mixture is stirred at rt for 4 hours, and then washed with diethyl ether (2×75 ml). The aqueous layer is cooled to 0° C., acidified to pH 1-2 and extracted with CH2Cl2. The organic phase is dried over MgSO4, filtered and concentrated to dryness to give the title compound (2S)-2-[methoxycarbonyl(methyl)amino]-3-methyl-butanoic acid (5.12 g, 71%) as a clear oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08779156B2 |
| 출처 데이터셋 | uspto-grants-2014_07 |
| ORD ID | ord-0e144cec5c7d415a837449b592c9b4e0 |
| 출처 메모 | uspto-grants-2014_07 |