関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Chloro-4-nitrobenzene | HCID 7474 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | HCID 178447845 | HCID 178447845 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | HCID 178447844 | HCID 178447844 | 76.1% |
反応手順
DMSO (300 ml) and KOH (38.0 g) were added to 1,1-bis(4-hydroxyphenyl)-4-(trans-4-n-propylcyclohexyl)cyclohexane (110.6 g) obtained in the first step, followed by dissolving these together on heating to 65° C., dropwise adding to the solution, a solution of p-chloronitrobenzene (97.8 g) in DMSO (500 ml) at 65° C., reacting the mixture, aging for 5 hours, cooling down to room temperature after completion of the reaction, extracting with dichloromethane, washing with lN-NaOH aqueous solution and further with saturated NaCl aqueous solution till the aqueous solution became neutral, drying over MgSO4, treating by alumina column, distilling off the resulting eluate and recrystallizing the resulting concentrate from a mixed solvent of toluene-acetone to obtain pale yellow crystals of 1,1-bis[4-(4-nitrophenoxy)phenyl]-4-(trans-4-n-propylcyclohexyl)cyclohexane (136.1 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05152918 |
|---|
| 出典データセット | uspto-grants-1992_10 |
|---|
| ORD ID | ord-d21098bb0785447ca17a5d309741bb2e |
|---|
| 出典メモ | uspto-grants-1992_10 |
|---|