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3-Chloro-1,2-propanediol → 1-(2,3-Dihydroxypropyl)-3-ethylimidazolium Chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloro-1,2-propanediol | HCID 7290 | — |
| 反応物 | 1-Ethyl-1H-imidazole | HCID 81540 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(2,3-Dihydroxypropyl)-3-ethylimidazolium Chloride | HCID 86668265 | 94.5% |
反応手順
1-Ethylimidazole (2.40 g, 25.0 mmol) and 3-chloro-1,2-propanediol (2.76 g, 25.0 mmol) were stirred in a 130° C. oil bath for 48 h, after which the flask was placed under vacuum and stirring continued at 130° C. for another 48 h. The residue was then dissolved in CH3OH, transferred to a tared flask and concentrated to afford the product as a viscous brown oil (4.88 g, 94%). 1H NMR: δH ppm (400 MHz; DMSO-d6) 1.41 (t, J=7.24 Hz, 3H) 3.23 (dd, J=11.17, 6.96 Hz, 1H) 3.37-3.47 (m, 1H) 3.70-3.86 (m, 1H) 4.11 (dd, J=13.74, 7.69 Hz, 1H) 4.22 (q, J=7.33 Hz, 2H) 4.33 (dd, J=13.74, 3.11 Hz, 1H) 5.19 (br. s., 1H) 5.59 (br. s., 1H) 7.78 (t, J=1.74 Hz, 1H) 7.85 (t, J=1.74 Hz, 1H) 9.33 (t, J=1.56 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09446348B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-c899e1ac34504b408478e6a345cdc370 |
| 出典メモ | uspto-grants-2016_09 |