Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
5-Fluoro-2-nitrophenol → cis-4-Fluoro-2-(2-methoxy-cyclohexyloxy)-1-nitro-benzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 5-Fluoro-2-nitrophenol | HCID 9937 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Cyclohexanol, 2-methoxy- | HCID 102911 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | cis-4-Fluoro-2-(2-methoxy-cyclohexyloxy)-1-nitro-benzene | HCID 67382391 | — |
반응 단계
2.36 ml DEAD were added to an ice-cooled solution of the 1.57 g 5-fluoro-2-nitrophenol, 1.95 ml 2-methoxycyclohexanol and 3.93 g triphenylphosphine in 30 ml THF. The reaction mixture was allowed to warm to rt overnight. The mixture was stirred additional 48 hours. Then the reaction mixture was diluted with methylene chloride and washed with 10% aq. potassium carbonate solution. The organic phase was passed through a hydrophobic frit and evaporated. Purification was achieved by silica gel column chromatography (solvent:10:1 iso-hexane: EtOAc).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08754079B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-427f75dbc9b24be0a9dd8076790ea3f4 |
| 출처 메모 | uspto-grants-2014_06 |