Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → tert-Butyl 3-(2-methylsulfanylethyl)-2-oxo-1,4,8-triazaspiro[4,5]decane-8-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | tert-Butyl 2-oxopiperidine-1-carboxylate | HCID 7577838 | — |
| 반응물 | (2S)-2-amino-4-(methylsulfanyl)butanamide hydrochloride | HCID 18531008 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | tert-Butyl 3-(2-methylsulfanylethyl)-2-oxo-1,4,8-triazaspiro[4,5]decane-8-carboxylate | HCID 68838394 | — |
반응 단계
N-tert-Butyloxycarbonylpiperidone (5.9 g, 29.8 mmol) and triethylamine (3.02 g, 29.8 mmol) were added to a solution of methioninamide hydrochloride (5.5 g, 29.8 mmol) in dry EtOH (66 ml), and the mixture was heated under reflux for 2.5 h. After addition of water (50 ml) and CH2Cl2 (200 ml), the organic phase was separated off, and the aqueous phase was extracted with CH2Cl2 (3×20 ml). The combined organic phases were dried over Na2SO4. After filtration, the solvent was removed by distillation. tert-Butyl 3-(2-methylsulfanylethyl)-2-oxo-1,4,8-triazaspiro[4,5]decane-8-carboxylate was obtained in a yield of 8.0 g (82% of theory).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07560468B2 |
| 출처 데이터셋 | uspto-grants-2009_07 |
| ORD ID | ord-6ae4bf239cf74b64a8df3a14ca157885 |
| 출처 메모 | uspto-grants-2009_07 |