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Water → 4,4'-Dimethylbenzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | P-Toluic Acid | HCID 7470 | — |
| 反応物 | Praseodymium(III) trifluoromethanesulfonate | HCID 9894708 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4,4'-Dimethylbenzophenone | HCID 69148 | 18.1% |
反応手順
Praseodymium (III) trifluoromethanesulfonate (3.53 g as a wet solid) and para-toluic acid (1.36 g) were refluxed together in 125 mL toluene with azeotropic removal of the lower water layer (Dean-Stark apparatus). After 24 hours, the mixture was cooled and extracted with 3×25 mL water, then by 2×25 mL saturated sodium bicarbonate solution. The organic layer was dried using anhydrous sodium sulfate, filtered, then concentrated down in vacuo to give crude 4,4′-dimethylbenzophenone (0.65 g, 31% yield) as a cream-colored crystalline solid. This was then recrystallized from methanol to give white needles of pure 4,4′ dimethylbenzophenone (0.19 g,9% yield) (M.P. 90.5-91.5° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06362375B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-e8bb410232d84efabe6c885972ec62d6 |
| 出典メモ | uspto-grants-2002_03 |