Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 3-({[tert-Butyl(diphenyl)silyl]oxy}methyl)-1-(2-chloro-4-nitrophenyl)pyridin-2(1H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Chloro-1-fluoro-4-nitrobenzene | HCID 67688 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | 3-({[tert-Butyl(diphenyl)silyl]oxy}methyl)pyridin-2(1H)-one | HCID 59410156 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-({[tert-Butyl(diphenyl)silyl]oxy}methyl)-1-(2-chloro-4-nitrophenyl)pyridin-2(1H)-one | HCID 59410186 | — |
반응 단계
At 0° C., 0.500 g (4.46 mmol) of potassium tert-butoxide is added to 1.08 g (2.97 mmol) of the compound from Example 3A in 21 ml of DMF, and the mixture is stirred at room temperature for 30 min. 0.571 g (3.27 mmol) of 2-chloro-1-fluoro-4-nitrobenzene is added, and the mixture is stirred at RT. After 4.5 h, 200 ml of water are added, and the mixture is then extracted three times with ethyl acetate. The combined organic phases are washed with water and then dried over sodium sulphate. After filtration, the solvents are removed under reduced pressure. The residue is purified by chromatography on silica gel (cyclohexane/ethyl acetate 9:1). This gives 872 mg (56% of theory) of the desired compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846934B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-445897fbd85c41d594077132b150d2ba |
| 출처 메모 | uspto-grants-2014_09 |