Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-(Ethylthio)ethanol → ethyl 3-(4-{(4-{4-[2-(ethylthio)ethoxy]-2,6-dimethylphenyl}-2,3-dihydro-1H-inden-1-yl)[(2-nitrophenyl)sulfonyl]amino}-2-fluorophenyl)propanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-(Ethylthio)ethanol | HCID 8075 | — |
| 반응물 | Tributylphosphine | HCID 13831 | — |
| 반응물 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 반응물 | ethyl 3-(2-fluoro-4-{[4-(4-hydroxy-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yl][(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate | HCID 23157316 | — |
| 용매 | Diisopropyl Ether | HCID 7914 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | ethyl 3-(4-{(4-{4-[2-(ethylthio)ethoxy]-2,6-dimethylphenyl}-2,3-dihydro-1H-inden-1-yl)[(2-nitrophenyl)sulfonyl]amino}-2-fluorophenyl)propanoate | HCID 23157179 | 93.1% |
반응 단계
To a solution of ethyl 3-(2-fluoro-4-{[4-(4-hydroxy-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yl][(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate (1.00 g, 1.58 mmol), 2-(ethylthio)ethanol (0.219 mg, 2.06 mmol) and tributylphosphine (0.417 mg, 2.06 mmol) in tetrahydrofuran (25 mL) was added 1,1′-(azodicarbonyl)dipiperidine (0.520 g, 2.06 mmol) under stirring at room temperature, and the mixture was stirred for 16 hr. The reaction mixture was diluted with diisopropyl ether, the insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (10%-80% ethyl acetate/hexane) to give the title compound (1.06 g, yield 93%) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07786165B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-69ec99ab814840ae97ded1f4294962f9 |
| 출처 메모 | uspto-grants-2010_08 |