Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dibromomethane → 2-[1,3]-Dithietan-2-ylidene-1-(3-nitro-phenyl)-2-pyridin-4-yl-ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dibromomethane | HCID 3024 | — |
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-(3-Nitro-phenyl)-2-pyridin-4-yl-ethanone | HCID 46929180 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-[1,3]-Dithietan-2-ylidene-1-(3-nitro-phenyl)-2-pyridin-4-yl-ethanone | HCID 46929181 | 76.3% |
반응 단계
To a solution of 1-(3-nitro-phenyl)-2-pyridin-4-yl-ethanone (5 g, 20.64 mmol) in dry DMSO (80 mL) under nitrogen atmosphere solid potassium carbonate (8.56 g, 61.92 mmol, 3 eq) was added at room temperature, followed by carbon disulfide (3.73 mL, 61.92 mmol, 3 eq) and dibromomethane (4.35 mL, 61.92 mmol, 3 eq). The reaction mixture was stirred at room temperature for 1 hour and then poured into stirred iced water (600 mL). The orange precipitate was filtered, washed with water and dried at 60° C. under reduced pressure for 1 hour. The crude product was purified by silica gel chromatography (SP1, eluant: n-hexane/ethyl acetate 2:8) to obtain 5.2 g of yellow solid (76%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524707B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-984c6d233822464a81856368e0122b59 |
| 출처 메모 | uspto-grants-2013_09 |