関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Salicylic Acid | HCID 338 | — |
| 反応物 | Lactic Acid | HCID 612 | — |
| 反応物 | Phosphonium, tetrabutyl-, hydroxide (1:1) | HCID 84487 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | HCID 178473643 | HCID 178473643 | — |
反応手順
Lactic acid (0.4504 g, 5 mmol), salicylic acid (0.6909 g, 5 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone and stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried at 0.01 mbar with stirring for 24 hrs. The desired compound is isolated as a colourless liquid; 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.63 (dd, J1=7.6 Hz, J2=1.9 Hz), 7.11 (m, 1H), 6.58 (m, 3H), 4.03 (q, J=6.9 Hz, 1H), 2.17 (m, 8H), 1.42 (m, 16 H), 1.23 (d, 7.0 Hz, 3H), 0.90 (t, J=7.3 Hz, 12 H). 31P-NMR (121.5 MHz, d6-DMSO) δ(ppm)=35.0. 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=176.3, 171.1, 163.0, 131.2, 129.9, 120.5, 117.8, 115.767.3, 23.4 (d, J=15.8 Hz), 22.6 (d, J=4.3 Hz), 20.5, 17.3 (d, J=47.7 Hz), 13.3 (s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09278134B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-0260974b33fc4dec97a88a0eb2af9a0b |
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| 出典メモ | uspto-grants-2016_03 |
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