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Potassium Carbonate → Ethyl 2-[2-(t-butyloxy)-2-oxo-ethoxy]-5-formylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | tert-Butyl bromoacetate | HCID 79177 | — |
| 反応物 | Ethyl 5-formyl-2-hydroxybenzoate | HCID 18930679 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 2-[2-(t-butyloxy)-2-oxo-ethoxy]-5-formylbenzoate | HCID 18930723 | 97.3% |
反応手順
Phenol 2c (1.0 g, 5.2 mmol), t-butyl bromoacetate (0.84 mL, 5.2 mmol), and potassium carbonate (0.79 g, 5.7 mmol) were heated at 65° C. in DMF (8 mL) overnight. After solvent removal, the mixture was diluted with EtOAc and extracted with water (3×), then brine. Drying (MgSO4) and removal of solvent gave a clear yellow oil (1.56 g). 1H-NMR(300 MHz, CDCl3): 9.93 (s, 1H), 8.35 (d, 1H, J=2 Hz), 7.99 (dd, 1H, J=9,2 Hz), 6.95 (d, 1H, J=9 Hz), 4.71 (s, 2H), 4.41 (q, 2H, J=7 Hz), 1.48 (t, 3H, J=7 Hz). Anal. Calc'd for C16H20O6 : C, 62.33; H, 6.54; Found: C, 62.05; H, 6.58.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05523302 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-aac7ab95d27c41d1a38bb201c3bb4d7a |
| 出典メモ | uspto-grants-1996_06 |