関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | 2-Allylphenol | HCID 15624 | — |
| 反応物 | 4-Fluorobenzophenone | HCID 67663 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[o-(1-Propenyl)phenoxy]benzophenone | HCID 54415597 | — |
反応手順
o-Allylphenol (33.5 g), 4-fluorobenzophenone (50.05 g), potassium carbonate (24.20 g), dry N-methylpyrrolidone (160 ml) and toluene (60 ml) are placed in a 3-necked 500 ml flask fitted with a stirrer, reflex condensor and thermometer and the mixture is heated under nitrogen to a temperature between 155°-160° C. and stirred for 3 hours. Water and toluene are separated via a Dean Stark trap and finally after 3 hours the reaction mixture reaches a temperature of 160° C. The mixture is cooled to 100° C. and a 1:1 mixture of toluene/water (400 ml) is added while stirring. After phase separation the aqueous layer is washed with toluene (50 ml) and the combined toluene layers are washed 4 times with water (150 ml). The toluene phase is dried over sodium sulphate and toluene distilled off by use of a rotary evaporator finally in vacuum leaving 4-[o-(1-propenyl)phenoxy]benzophenone as a light yellow melt. The yield is 73 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04789704 |
|---|
| 出典データセット | uspto-grants-1988_12 |
|---|
| ORD ID | ord-33fb45e1eee9447baa9e133e19e2a1bc |
|---|
| 出典メモ | uspto-grants-1988_12 |
|---|