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Water → (4-Methoxyphenyl)(4-methylphenyl)methanone
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 | Anisole | HCID 7519 | — |
| 触媒 | Hafnium(IV) Trifluoromethanesulfonate | HCID 9853707 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | (4-Methoxyphenyl)(4-methylphenyl)methanone | HCID 32113 | 9% |
反応手順
Hafnium (IV) trifluoromethanesulfonate (5.15 g), anisole (1.08 g) and para-toluic acid (1.36 g) were refluxed together in 125 mL chlorobenzene with azeotropic removal of the upper water layer (inverse Dean-Stark apparatus). After 3 hours, the mixture was cooled and extracted with 2×25 mL water, then 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-methoxy-4′-methylbenzophenone (0.20 g, 9% yield) as a colored crystalline solid. The aqueous layer was concentrated in vacuo to give 4.41 g of a damp, white solid.
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-9a2ab42f81ea45869a220583f5a397ed |
| 出典メモ | uspto-grants-2002_03 |