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Salicylic Acid → HCID 178454881、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Salicylic Acid | HCID 338 | — |
| 反応物 | Phosphonium, tetrabutyl-, hydroxide (1:1) | HCID 84487 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | HCID 178454881 | HCID 178454881 | — |
反応手順
Salicylic acid (5-20 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.) with stirring for 24 hrs. 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.74 (dd, J1=7.7 Hz, J2=1.9 Hz, 1H), 7.32 (dt, J1=7.6 Hz, J2=1.8 Hz, 1H), 6.8 (m, 2H), 2.20 (m, 4 H), 1.41 (m, 8 H), 0.9 (t, J=7.1 Hz, 6 H). 31P-NMR (121.5 MHz, d6-DMSO) δ(ppm)=35.1. 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=171.9(s), 163.1(s), 131.1 (d), 129.8(d), 120.6 (s), 115.7 (d), 115.6 (d), 23.3 (d, J=16.4 Hz), 22.6 (d, J=4.8 Hz), 17.3 (d, J=47.3 Hz), 13.2 (s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09278134B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-79fdd7867a444a6eb52723b3abf9171b |
| 出典メモ | uspto-grants-2016_03 |