Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Propyl chloroformate | HCID 7998 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 3-[2-(Trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-one | HCID 50943475 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one | HCID 67458997 | 68.2% |
반응 단계
3-[2-(Trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-one (0.13 g, 0.38 mmol) and sodium hydrogen carbonate (0.06 g, 0.71 mmol) was suspended in acetonitrile (15 ml), added with propyl chloroformate (0.09 g, 0.77 mmol) and heated to reflux for six hours. After cooling to room temperature, the reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4) to obtain 3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one (0.11 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08048825B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-6b8d7d689bc74860aaa9e3e40448eaac |
| 출처 메모 | uspto-grants-2011_11 |