関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-Chloro-4-ethoxyneophyl 3-phenoxybenzyl ether | HCID 3067183 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether | HCID 11058070 | 48.9% |
反応手順
One hundred grams of 3-phenoxybenzyl 2-(3-chloro-4-ethoxyphenyl)-2-methylpropyl ether and 25 g of potassium hydroxide were added to 300 ml of 1,3-dimethyl-2-imidazolidinone (to be abbreviated as DMI hereinafter), and the mixture was stirred at 150° C. for hours. The reaction mixture was cooled to room temperature, poured into water, acidified with a concentrated hydrochloric acid, and extracted with benzene. The benzene solution was washed with water, and dried. Benzene was evaporated under reduced pressure. The resulting oily residue was purified by column chromatography (silica gel; eluent: benzene) to give 45.6 g 3-phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether having a melting point of 68° to 69° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04782094 |
|---|
| 出典データセット | uspto-grants-1988_11 |
|---|
| ORD ID | ord-70c81f49e2d8426e8d2edacebf1895b2 |
|---|
| 出典メモ | uspto-grants-1988_11 |
|---|