関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1-Bromododecane | HCID 8919 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Pyrrolidone | HCID 12025 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 触媒 | Dihydroxy(dioxo)molybdenum;phosphonic acid | HCID 21863154 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 1-Lauryl-2-pyrrolidone | HCID 62459 | 80% |
反応手順
Step A is conducted by adding tetrabutylammonium bromide (950 mg-3 mmol-0.05 eq.) and powder potash (23.1 g-411 mmol-7 eq.) under agitation to a solution of 2-pyrrolidinone (5.00 g-58.8 mmol) and bromododecane (18.5 mL, 76.4 mmol, 1.3 eq.) in toluene (60 mL). The mixture is heated to 50° C. overnight. After disappearance of the 2-pyrrolidinone (verified by TLC using a 4:1 v/v mixture of ethyl acetate and cyclohexane, and phosphomolybdic acid for detection) and cooling, 60 mL of water is added and the mixture left under agitation for a further 15 minutes. The aqueous and organic phases are separated and the aqueous phase is extracted once with diethylether (60 mL). The organic phases are combined, dried over Na2SO4, filtered and concentrated. After vacuum distillation (146° C.-0.5 mbars), N-dodecylpyrrolidin-2-one is obtained (Yield: 80%) for which the 1H and 13C NMR characterisations are as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09441285B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-7baa9a23c78d44c88ef74d641bd2c050 |
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| 出典メモ | uspto-grants-2016_09 |
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