Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dibromomethane → 3-(2-[1,3]Dithietan-2-ylidene-2-pyridin-4-yl-acetyl)-benzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dibromomethane | HCID 3024 | — |
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-(Pyridin-4-yl-acetyl)-benzonitrile | HCID 67184353 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-(2-[1,3]Dithietan-2-ylidene-2-pyridin-4-yl-acetyl)-benzonitrile | HCID 22944123 | 58.1% |
반응 단계
To a solution of 3-(pyridin-4-yl-acetyl)-benzonitrile (12.5 g, 56 mmol) in dry DMSO (280 mL) under nitrogen atmosphere solid potassium carbonate (23.36 g, 169 mmol, 3 eq) was added at room temperature, followed by carbon disulfide (10.2 mL, 169 mmol, 3 eq) and dibromomethane (11.86 mL, 169 mmol, 3 eq). The reaction mixture was stirred at room temperature for 2 hours and then poured into stirred iced water (1.5 L 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 10.1 g of yellow solid (58%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524707B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-4e457fb01b9a4e2facf6d9dcb4d89066 |
| 출처 메모 | uspto-grants-2013_09 |