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Methane → 3-Amino-1-chloro-3-methylpentan-2-one hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 3-Amino-1,1-dichloro-3-methyl-2-pentanone hydrochloride | HCID 18372006 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Amino-1-chloro-3-methylpentan-2-one hydrochloride | HCID 18372002 | 196.6% |
反応手順
In a 2 L Parr bottle were placed 41 g of 3-amino-1,1-dichloro-3-methyl-2-pentanone hydrochloride, 0.8 g of 10% palladium over charcoal and 400 ml of ethanol (200 proof). The resulting mixture was shaken in a Parr apparatus at 50 psi for 3 hours. The crude reaction mixture was filtered through Celite™ filter agent and evaporated in vacuo. A viscous oil resulted, which was taken up in approximately 400 ml of ethyl acetate and stirred at room temperature for several hours. The expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride crystallized as a white solid. To the resulting suspension were added 300 ml of hexane. Filtration yielded 34 g (98%) of the expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride (Compound 14).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05929098 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-bfe75ec575e94cd696b03ae05edf33da |
| 出典メモ | uspto-grants-1999_07 |