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Potassium Iodide → 1-Dodec-7-ynyl-4-methyl-pyridinium iodide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 4-Methylpyridine | HCID 7963 | — |
| 反応物 | 12-Chloro-5-dodecyne | HCID 123509 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 1-Dodec-7-ynyl-4-methyl-pyridinium iodide | HCID 24781248 | 87% |
反応手順
12-Chloro-dodec-5-yne (1 mmol) was mixed with potassium iodide (3 mmol) and 4-picoline (3 mmol) in butanone. The mixture was refluxed for 3 days and cooled to room temperature, filtrated. The butanone was removed in a vacuum, and the resulting residue was partitioned between water and ethyl ether. The aqueous layer was washed extensively with ether until no 4-picoline was left in the aqueous layer. The resulting aqueous solution of the product was extracted with chloroform. The chloroform was removed to afford the product (87%). 1HNMR (300 MHz, CDCl3, ppm), 9.28 (d, 2H), 7.92 (d, 2H), 4.92 (t, 2H), 2.68 (s, 3H), 1.96-2.18 (m, 6H), 1.32-1.50 (br, 10H), 0.88 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846937B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b0bfcadd460f456794c4379eb17c286d |
| 出典メモ | uspto-grants-2014_09 |