Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → tert-Butyl 4-sulfanylpiperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | tert-Butyl 4-(acetylthio)piperidine-1-carboxylate | HCID 22494773 | — |
| 반응물 | Sodium methanolate methanol | HCID 23694274 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | tert-Butyl 4-sulfanylpiperidine-1-carboxylate | HCID 21906090 | 98.9% |
반응 단계
In dry methanol were dissolved 520 mg (2 mmol) of 4-(acetylthio)-1-(tert-butoxycarbonyl)piperidine, and 420 μl (2 mmol) of a 28% sodium methoxide-methanol solution were added to the mixture under ice-cooling and under a nitrogen atmosphere, followed by stirring of the resulting mixture for 40 minutes. Then, 173 μl of acetic acid were added to the mixture and the solvent was distilled off at room temperature, followed by diluting of the residue with ethyl acetate. The mixture was washed successively with an aqueous sodium hydrogencarbonate solution and an aqueous NaCl solution in the order and the solvent was distilled off to obtain 430 mg of reddish orange oil. This product was used for a subsequent reaction without purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06300357B1 |
| 출처 데이터셋 | uspto-grants-2001_10 |
| ORD ID | ord-6e02e78c80f640369042e7db9c28b062 |
| 출처 메모 | uspto-grants-2001_10 |