참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | 2,4-Dimethylpyridine | HCID 7936 | — |
| 반응물 | 12-Chloro-5-dodecyne | HCID 123509 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | 1-Dodec-7-ynyl-2,4-dimethyl-pyridinium iodide | HCID 24781250 | 84% |
반응 단계
12-Chloro-dodec-5-yne (1 mmol) was mixed with potassium iodide (3 mmol) and 2,4-lutidine (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 2,4-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 (84%). 1HNMR (300 MHz, CDCl3, ppm), 9.40 (d, 1H), 7.75 (d, 1H), 7.66 (s, 1H), 4.78 (t, 3H), 2.88 (s, 3H), 2.60 (s, 3H), 2.05-2.15 (br, 4H), 1.80-2.00 (br, 2H), 1.30-1.50 (br, 10H), 0.86 (t, 3H); 13CNMR, 156.73, 153.05, 145.84, 136.61, 127.27, 80.86, 79.85, 58.12, 31.54, 30.94, 39.09, 26.17, 22.39, 22.30, 21.03, 18.96, 18.79, 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-78cdc0c3a89046eb95004dcc3b89588b |
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| 출처 메모 | uspto-grants-2014_09 |
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