참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Bromothiophenol | HCID 66049 | — |
| 반응물 | 1,3-Difluoro-5-iodobenzene | HCID 2778221 | — |
| 반응물 | Heptanedione, tetramethyl- | HCID 11191887 | — |
| 촉매 | Cuprous chloride | HCID 62652 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | HCID 86694942 | HCID 86694942 | 78.2% |
반응 단계
N-Methyl-2-pyrrolidone (10 mL) was added to 4-bromothiophenol (0.500 g, 2.64 mmol) in a sealed tube and the mixture was purged with argon for 5 minutes. After this time, 3,5-difluoroiodobenzene (0.63 g, 2.64 mmol), CuCl (0.131 g, 1.32 mmol), tetramethyl heptanedione (0.14 mL, 0.66 mmol) and cesium carbonate (1.70 g, 5.28 mmol) were added to the reaction mixture. The reaction mixture was stirred at 130° C. under argon for 2 hours. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, and filtered through a celite bed. The filtrate was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to yield the crude product. Silica gel chromatography (neat hexanes) provided impure 1-(4-bromo-phenylsulfanyl)-3,5-difluorobenzene (0.622 g). MS calcd. for C12H8BrF2S [(M+H)+] 302, obsd. 302.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09000044B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_04 |
|---|
| ORD ID | ord-7c4dda7f90cf43afa3c05578424fa0a5 |
|---|
| 출처 메모 | uspto-grants-2015_04 |
|---|