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Potassium Carbonate → 1-(4-(2-(Diethylamino)ethoxy)phenyl)butan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-2-(diethylamine)ethane hydrochloride | HCID 13363 | — |
| 反応物 | 1-Butanone, 1-(4-hydroxyphenyl)- | HCID 66092 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(4-(2-(Diethylamino)ethoxy)phenyl)butan-1-one | HCID 66822369 | 98.8% |
反応手順
2-(Diethylamino)ethyl chloride hydrochloride (624 mg, 3.65 mmol) was added to a stirred solution of p-hydroxybutyrophenone (200 mg, 1.21 mmol) in anhydrous acetone (6 mL) followed by the addition of potassium carbonate (668 mg, 4.84 mmol). The resulting mixture was heated at reflux for 48 hours. The mixture was diluted with ethyl acetate, washed with water (2×) and sat. brine, dried over sodium sulfate, and concentrated to an oil. Flash silica gel column chromatography, eluting with 1:1 hexanes/ethyl acetate, afforded 21 (315 mg, 98%) as a light yellow oil: MS (ES+) m/z 264.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08809377B2 |
| 出典データセット | uspto-grants-2014_08 |
| ORD ID | ord-e46f2f20693e44b7b8d6e43fb387b48a |
| 出典メモ | uspto-grants-2014_08 |