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Hexane → Zoxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3,5-Dichloro-4-methylbenzoyl chloride | HCID 11127919 | — |
| 反応物 | 3-Amino-1-chloro-3-methylpentan-2-one hydrochloride | HCID 18372002 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Zoxamide | HCID 122087 | 60.5% |
反応手順
To a well-stirred solution of 1.1 g (13.1 mmol) sodium bicarbonate in 15 mL water was added solid 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride (1 g, 5.4 mmoles) portionwise. To the resulting solution was added 15 mL of hexane followed by dropwise addition of a solution of 3,5-dichloro-4-methylbenzoyl chloride (1.2 g, 5.4 mmol) in 1 mL of tetrahydrofuran. Another 15 mL of hexane was added, and the resulting mixture was stirred at room temperature for 2 hours. The reaction mixture was filtered, and the resulting white solid was dried in a vacuum oven yielding 1.1 g of 3,5-dichloro-N-(3-chloro-1-ethyl-1-methyl-2-oxopropyl)-4-methylbenzamide as a white solid (mp 159°-161° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05874466 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-af42f171e3c64c44b3173bf4bd5cd1da |
| 出典メモ | uspto-grants-1999_02 |