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Diethyl Ether → 4-[N-(benzylidene)aminomethyl]-1-(2-pyridinesulphonyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pyridine-2-sulfonyl Chloride | HCID 3787675 | — |
| 反応物 | N-Benzylidene(piperidin-4-yl)methanamine | HCID 11820173 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[N-(benzylidene)aminomethyl]-1-(2-pyridinesulphonyl)piperidine | HCID 23284888 | 68.4% |
反応手順
Triethylamine (6.3 ml) was added to a cloudy solution of N-benzylidene-4-piperidylmethylamine (4.05 g) and pyridine-2-sulphonyl chloride (4.0 g) in dichloromethane (100 ml) and the resulting clear yellow solution was stirred for 14 hours. Removal of the solvent under reduced pressure gave a yellow solid which on addition of diethyl ether (100 ml) partly dissolved. The insoluble white solid (triethylamine hydrochloride) was removed by filtration. Evaporation of the filtrate afforded a flocculent yellow solid which recrystallised from ethanol to give 4-[N-(benzylidene)aminomethyl]-1-(2-pyridinesulphonyl)piperidine as a white crystalline solid (4.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06136825 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-af024818ab744dabafd169752ca52401 |
| 出典メモ | uspto-grants-2000_10 |