Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium → (5-Fluoro-2-phenoxy-phenyl)-{5-methoxy-2-[2-(mesyloxy-)-ethoxy]-benzyl}-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium | HCID 5360545 | — |
| 반응물 | 5-Fluoro-2-phenoxyaniline | HCID 19627132 | — |
| 반응물 | 5-Methoxy-2-(2-mesyloxyethoxy)-benzaldehyde | HCID 59765855 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,1-Dichloroethane | HCID 6365 | — |
| 생성물 | (5-Fluoro-2-phenoxy-phenyl)-{5-methoxy-2-[2-(mesyloxy-)-ethoxy]-benzyl}-amine | HCID 86621787 | 62% |
반응 단계
To stirred solution of 9.1 g (45 mmol) 1b, 12.3 g (45 mmol) 4a and one drop of glacial acid in 60 ml dichloroethane (pH=5) were added 14.8 g (70 mmol) sodium tris-acetoxy hydro borane. The reaction mixture was stirred over night and diluted with 5 ml water. The pH value was adjusted with aqueous sodium hydroxyd solution to pH=8-9. The mixture was extracted three times with dichloromethane. The combined organic phases were washed with water and brine and were dried with magnesium sulfate. The desired crude product 4b was obtained in 62% yield (12.9 g, 27.9 mmol) as yellow oil. The crude product 4b was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07803960B2 |
| 출처 데이터셋 | uspto-grants-2010_09 |
| ORD ID | ord-787d6f34270a46d5a6eeb4857bbad118 |
| 출처 메모 | uspto-grants-2010_09 |