참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | 3,4-Dimethylpyridine | HCID 11417 | — |
| 반응물 | 12-Chloro-5-dodecyne | HCID 123509 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | 1-Dodec-7-ynyl-3,4-dimethyl-pyridinium iodide | HCID 24781254 | 72% |
반응 단계
12-Chloro-dodec-5-yne (1 mmol) was mixed with Sodium iodide (3 mmol) and 3,4-lutidine (3 mmol) in butanone. The mixture was refluxed for 3 days and cooled to room temperature, filtrated. The butanone was removed in vacuum, and the resulting residue was partitioned between water and ethyl ether. The aqueous layer was washed extensively with ether until no 3,4-lutidine 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 (72%). 1HNMR, (300 MHz, CDCl3, ppm, ppm), 9.22 (s, 1H), 9.04 (d, 1H), 7.80 (d, 1H), 4.84 (t, 3H), 2.52 (s, 3H), 2.50 (s, 3H), 1.92-2.14 (m, 6H), 1.28-1.45 (m, 10H), 0.84 (t, 3H). 13CNMR, 157.84, 143.39, 141.81, 138.53, 128.72, 80.80, 79.90, 61.23, 32.03, 31.54, 29.08, 28.48, 25.91, 22.30, 20.78, 18.96, 18.79, 17.44, 14.02.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846937B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-5e891cc7ab8f4e1186ceef63d022a235 |
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| 출처 메모 | uspto-grants-2014_09 |
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