関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propionyl chloride | HCID 62324 | — |
| 反応物 | N-phenyl-1-(2-phenylethyl)-4-piperidinamine | HCID 88890 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | Fentanyl | HCID 3345 | — |
反応手順
In two neck round bottom flask equipped with condenser pressure equalizing funnel and calcium chloride guard tube, a solution of 28.0 (0.10 moles) of 4-anilino N-phenethyl piperidine prepared in step II, in 150 ml of dichloroethane was taken. To this solution, 9.25 gm (0.10 moles) of propionyl chloride was added drop wise through pressure equalizing funnel with continuous stirring. After the completion of the addition, the mixture was further stirred for 10 hrs. After the completion of the reaction, the reaction mixture was washed with 20% sodium hydroxide solution. The aqueous phase was extracted with 2×100 ml of dichloromethane. The combined organic extract was dried over sodium sulphate and concentrated to give crude fentanyl. The crude product was recrystallised from petroleum ether (60 to 80° C.) to give colourless crystals of pure fentanyl having mp 82 to 83° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08399677B2 |
|---|
| 出典データセット | uspto-grants-2013_03 |
|---|
| ORD ID | ord-f66d9b4e924b4dcf8db083810bc19569 |
|---|
| 出典メモ | uspto-grants-2013_03 |
|---|