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Dibromomethane → 1-(3-Bromo-phenyl)-2-[1,3]dithietan-2-ylidene-2-pyridin-4-yl-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibromomethane | HCID 3024 | — |
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(3-Bromophenyl)-2-(pyridin-4-yl)ethan-1-one | HCID 53952423 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(3-Bromo-phenyl)-2-[1,3]dithietan-2-ylidene-2-pyridin-4-yl-ethanone | HCID 15485913 | 74% |
反応手順
1-(3-Bromo-phenyl)-2-pyridin-4-yl-ethanone (150 mg, 0.54 mmol), dibromomethane (114 ul, 1.62 mmol) and carbon disulfide (77 ul, 1.62 mmol) were reacted at room temperature in dry DMSO in the presence of K2CO3 (225 mg, 1.62 mmol) for three hours. The reaction, evaporated to dryness, was worked up with water and ethyl acetate. The pooled organic extracts were washed with brine, dried over sodium sulphate and evaporated down. The crude material was purified by a quick elution with ethyl acetate through a pad of silica to give the clean product in 74% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524707B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-9d9771a2591945309c5b19668224ff47 |
| 出典メモ | uspto-grants-2013_09 |