Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfoxide → tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Sulfoxonium, trimethyl-, iodide (1:1) | HCID 74498 | — |
| 반응물 | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate | HCID 22135564 | 80.3% |
반응 단계
55% sodium hydride (6.02 g) was added under ice-cooling to a DMSO (250 mL) suspension of trimethylsulfoxonium iodide (33.1 g), and stirring was performed at room temperature for 1 hour. A DMSO (125 ml) solution of tert-butyl 4-oxopiperidine-1-carboxylate (25.0 g) was added, and heated and stirred at 60° C. for 1 hour. Purified water was added to the mixture, and extraction was performed with EtOAc. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (EtOAc/hexane) to obtain tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate (21.5 g),
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822688B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-7a1082cecff047baad1b5aa5230fb810 |
| 출처 메모 | uspto-grants-2014_09 |