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Acetonitrile → 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)-1-[2-(1,4-benzodioxan-6-yl)ethyl]pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,2-Diphenyl-2-(pyrrolidin-3-yl)acetamide | HCID 13633754 | — |
| 反応物 | 6-(2-Bromoethyl)-2,3-dihydro-1,4-benzodioxin | HCID 19088508 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)-1-[2-(1,4-benzodioxan-6-yl)ethyl]pyrrolidine | HCID 19746811 | — |
反応手順
A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.3 g--see Preparation 8), 6-(2-bromoethyl)-1,4-benzodioxan (0.26 g--see Preparation 21), anhydrous potassium carbonate (0.4 g) and acetonitrile (10 ml) was heated under reflux for 3 hours. On cooling to room temperature, water (40 ml) was added and the mixture was extracted with dichloromethane (3×30 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a foam which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 10%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a colourless foam, yield, 0.21 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05096890 |
| 出典データセット | uspto-grants-1992_03 |
| ORD ID | ord-feb6f498224948d98b4b3ba45295b1f7 |
| 出典メモ | uspto-grants-1992_03 |