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4-(Naphthalen-2-yl)piperidine → (S)-alpha-(2'-(2-Hydroxy-3-(4-(naphthalen-2-yl)piperidino)propyloxy)benzylidene)-gamma-butyrolactone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-(Naphthalen-2-yl)piperidine | HCID 22029264 | — |
| 反応物 | (S)-alpha-(2'-(2,3-epoxypropan-1-yloxy)benzylidene)-gamma-butyrolactone | HCID 86585643 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (S)-alpha-(2'-(2-Hydroxy-3-(4-(naphthalen-2-yl)piperidino)propyloxy)benzylidene)-gamma-butyrolactone | HCID 69497913 | 53.8% |
反応手順
(S)-α-(2′-(2,3-epoxypropan-1-yloxy)benzylidene)-γ-butyrolactone (50 g) and 4-(naphthalen-2-yl)piperidine (43 g) were dissolved in ethanol (500 ml) and the mixture was refluxed under heating for 2 hr. After cooling, the solvent was evaporated under reduced pressure and the obtained crystals were collected by filtration. The crystals were recrystallized once from acetonitrile and once from a mixed solvent of ethyl acetate and ethanol to give the title compound (50 g), melting point 138–140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07196199B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-857f9eddc4a9439095e53212e9b9fd2f |
| 出典メモ | uspto-grants-2007_03 |