関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Dibromobutane | HCID 21508 | — |
| 反応物 | Tert-butyl 4-((4-aminophenoxy)methyl)piperidine-1-carboxylate | HCID 23366952 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Tert-butyloxycarbonyl-4-[(4-pyrrolidinophenyloxy)methyl]piperidine | HCID 23366966 | 62.3% |
反応手順
To 1-tert-butyloxycarbonyl-4-[(4-aminophenyloxy)methyl]piperidine (0.75 g) obtained in Example 13 were added dimethylformamide (10 ml), potassium carbonate (1.4 g) and dibromobutane (0.54 g) and the mixture was heated to 70° C. and stirred overnight. To the reaction solution was added water which was extracted with ethyl acetate (50 ml×3). The combined extract was dried over sodium sulfate and concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate=5/1 (v/v)) to obtain 1-tert-butyloxycarbonyl-4-[(4-pyrrolidinophenyloxy)methyl]piperidine (0.55 g) as colorless crystals, m.p. 141°-145° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05580883 |
|---|
| 出典データセット | uspto-grants-1996_12 |
|---|
| ORD ID | ord-30fb7d061a3c46b98cb0c872aa1589f6 |
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| 出典メモ | uspto-grants-1996_12 |
|---|
