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Dimethyl Sulfoxide → 1-(4-Methylbenzyl)piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 1-(4-Methylbenzyl)piperidin-4-ol | HCID 791482 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-Methylbenzyl)piperidin-4-one | HCID 11959541 | 81% |
反応手順
To 2.8 mL (32 mmol) of oxalyl chloride in 75 mL of CH2Cl2 at −78° C. was added 4.6 mL (64 mmol) of DMSO. To this mixture was added 5.3 g (26 mmol) of 1-(4-methylbenzyl)-4-piperidinol 123 in 10 mL of CH2Cl2, and the mixture was stirred 5 min in the cold. The mixture was quenched with 18 mL (129 mmol) of triethylamine and allowed to come to room temperature, and saturated aqueous ammonium chloride was added. The organic phase was washed with water and brine, dried, and evaporated to give 4.27 g (81%) of 1-(4-methylbenzyl)-4-piperidinone (124), which was used as is without further purification. GC/MS showed 100% purity with a molecular ion of 203.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06521622B1 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-4341698cc7444296979cce052115302a |
| 出典メモ | uspto-grants-2003_02 |