関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Iodopropane | HCID 33643 | — |
| 反応物 | 5-Chloro-2-(hydroxymethyl)phenol | HCID 327148 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 86725582 | HCID 86725582 | 58% |
反応手順
Charge 5-chloro-2-(hydroxymethyl)phenol (997 mg, 6.29 mmol, PREPARATION 7), iodopropane (1.17 g, 6.92 mmol), K2CO3 (1.74 g, 12.58 mmol) and DMF (6 mL) to a sealed tube. The reaction mixture was heated to 100° C. overnight. It was then poured into ice-water and extracted with ethyl acetate twice, washed the organic phase with water twice, brine and dried with Na2SO4, concentrated and purified by silica gel chromatograph to give the title compound (729 mg, 58%). 1H NMR (400 MHz, CDCl3): δ 1.05 (3H, t, J=7.2 Hz), 1.79-1.88 (2H, m), 3.96 (2H, t, J=6.4 Hz), 4.64 (2H, s), 6.85 (1H, d, J=1.2 Hz), 6.91 (1H, dd, J=1.6 Hz, 8.4 Hz), 7.20 (1H, d, J=8.0 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09107916B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-0d4dfb69545f4815926283b358c2a4fc |
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| 出典メモ | uspto-grants-2015_08 |
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