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Water → 3,3-Dimethylbutyl 3-piperidinopropyl ether
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 15-Crown-5 | HCID 36336 | — |
| 反応物 | 1-Chloro-3,3-dimethylbutane | HCID 76111 | — |
| 反応物 | HCID 23694275 | HCID 23694275 | — |
| 触媒 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3,3-Dimethylbutyl 3-piperidinopropyl ether | HCID 9794557 | — |
反応手順
Sodium 3-piperidinopropanolate (5 mmol), 5 mmol of 3,3-dimethylbutyl chloride, a catalytic amount of tetrabutylammonium iodide, and 0.5 mmol of 15-crown-5 in 10 ml of dry dimethyl sulfoxide were refluxed for 12 hours. Water was added, and it was extracted with diethyl ether. The organic layer was purified by column chromatography on silica gel (eluent: methylene chloride/methanol (90/10), ammonia atmosphere). The solvent was removed under reduced pressure and the residue crystallized with oxalic acid from diethyl ether/ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07910605B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-49afa6cd8b4744a28766d5e2c34b0174 |
| 出典メモ | uspto-grants-2011_03 |