関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 1-benzylpiperidine-4-carboximidate dihydrochloride | HCID 18670137 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 1-benzylpiperidine-4-carboximidate | HCID 18670138 | 101.2% |
反応手順
6.1 g of methyl 1-benzylpiperidine-4-carboximidate dihydrochloride was distributed into an aqueous solution of potassium carbonate and ethyl acetate under ice-cooling. The organic layer was extracted and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, 4.7 g of free methyl 1-benzylpiperidine-4-carboximidate was obtained as a colorless oily substance. A solution of 2.35 g of methyl 1-benzylpiperidine-4-carboximidate and 0.95 g (10 mmol) of methanesulfonamide in dry methanol was stirred at room temperature for 3 days. Subsequently, 1.0 g of palladium-carbon was added to the reaction mixture and the resulting mixture was stirred in a hydrogen atmosphere under atmospheric pressure for 1 hour. The inorganic matters were eliminated by filtering through celite. After distilling off the solvent under reduced pressure, the residue was recrystallized from methanol to thereby give 1.38 g of the title compound as colorless needles.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06518423B1 |
|---|
| 出典データセット | uspto-grants-2003_02 |
|---|
| ORD ID | ord-9802986a210a4a148a1c2f7d65882414 |
|---|
| 出典メモ | uspto-grants-2003_02 |
|---|