関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | L-Pyroglutamic Acid | HCID 7405 | — |
| 反応物 | Phosphonium, tetrabutyl-, hydroxide (1:1) | HCID 84487 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | tetrabutylphosphonium (S)-(-)-2-pyrrolidone-5-carboxylate | HCID 86626712 | 98% |
反応手順
5.0 g of (S)-(−)-2-pyrrolidone-5-carboxylic acid (by Wako Pure Chemical Industries) was suspended in 30 ml of methanol, and 26.8 g of aqueous 40% tetrabutylphosphonium hydroxide (by Aldrich) was dropwise added thereto at 0° C., taking 3 minutes. After being stirred for 10 minutes, this was concentrated under reduced pressure at 40° C., using an evaporator. 50 ml of methanol was added to the residue, and the mixture was concentrated under reduced pressure in the same manner. 100 ml of toluene was added to the obtained residue, and the resulting mixture was concentrated under reduced pressure; and this operation was repeated twice. Next, this was concentrated in ultra-high vacuum at from room temperature to 50° C. for 15 hours. 15.3 g of tetrabutylphosphonium (S)-(−)-2-pyrrolidone-5-carboxylate (purity, 98.0%) was obtained as an oily compound. (This is an ionic liquid A.) In NMR analysis, neither toluene nor methanol was detected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09018321B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-6454a0abcdf64cf5b9d29773a389a8cc |
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| 出典メモ | uspto-grants-2015_04 |
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