関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1-Dichloroethane | HCID 6365 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Stilbene | HCID 11502 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-Chloro-1-methyl-2,2-diphenylcyclopropane | HCID 12869608 | 78% |
反応手順
Under a nitrogen atmosphere, 1,1-dichloroethane (30.0 g, 303 mmol), diphenylethylene (5.59 g, 31.0 mmol) and diethyl ether (62 ml) were placed in a reaction flask and cooled to −40° C. To the mixture, n-butyllithium in hexane (45 ml, 1.56M, 70.2 mmol) was added gradually and the mixture was stirred at the same temperature for one hour, followed by warming to room temperature. Then, water was added to the reaction mixture and the organic layer was extracted with toluene. The toluene extract was dried over anhydrous magnesium sulfate and then the solvent was removed under reduced pressure. The concentrate was recrystallized from ethanol to give the title compound (5.91 g, 78%) as white crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07129367B2 |
|---|
| 出典データセット | uspto-grants-2006_10 |
|---|
| ORD ID | ord-b0bfc69739404093b84d5e3d93a8775d |
|---|
| 出典メモ | uspto-grants-2006_10 |
|---|