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Trimethylsilyl isocyanate → 4-(t-Butoxycarbonylamino)-1-(1-carbamoyl-4-piperidinylmethyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilyl isocyanate | HCID 70696 | — |
| 反応物 | 4-(t-Butoxycarbonylamino)-1-(4-piperidinylmethyl)piperidine | HCID 12986154 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(t-Butoxycarbonylamino)-1-(1-carbamoyl-4-piperidinylmethyl)piperidine | HCID 69830937 | 83.1% |
反応手順
To a solution of 4-(t-butoxycarbonylamino)-1-(4-piperidinylmethyl)piperidine (590 mg) in methylene chloride (30 ml) is added trimethylsilyl isocyanate (220 mg) under ice-cooling, and the mixture is stirred at room temperature for 8 hours. The reaction mixture is washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent is evaporated under reduced pressure. The residue is purified by silica gel column chromatography (eluent; chloroform:methanol=10:1) to give 4-(t-butoxycarbonylamino)-1-(1-carbamoyl-4-piperidinylmethyl)piperidine (540 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06294555B1 |
| 出典データセット | uspto-grants-2001_09 |
| ORD ID | ord-2324d1ff461043089d5299707662b91e |
| 出典メモ | uspto-grants-2001_09 |