Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 8-Benzyl-8-azaspiro[bicyclo[3.2.1]octane-3,2'-oxirane]
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Sulfoxonium, trimethyl-, iodide (1:1) | HCID 74498 | — |
| 반응물 | 8-Benzyl-8-azabicyclo(3.2.1)octan-3-one | HCID 119846 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 8-Benzyl-8-azaspiro[bicyclo[3.2.1]octane-3,2'-oxirane] | HCID 86659829 | — |
반응 단계
Trimethyl sulfoxonium iodide (3.07 g, 13.9 mmol) is placed in 18 ml of DMSO under nitrogen in the presence of sodium hydride dispersed at 60% in oil (0.56 g, 13.9 mmol). After stirring for 30 min at ambient temperature, 8-benzyl-8-aza-bicyclo[3.2.1]octan-3-one (2.0 g, 9.3 mmol) solubilized in 3 ml of DMSO is slowly added. The reaction medium is kept stirring for 4 h and then kept without stirring for 60 h, After hydrolysis, and extraction with ethyl acetate, the organic phase is washed with a saturated aqueous sodium chloride solution and dried over MgSO4. 2.04 g of 8-benzyl-spiro[8-azabicyclo[3.2.1]octane-3,2′-oxirane], subsequently used as it is, are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08530477B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-752f31fa474c4665ac632012bf329c96 |
| 출처 메모 | uspto-grants-2013_09 |