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Phenylglyoxylic Acid → N'-t-butyl-N'-benzoylcarbonyl-N-benzoylhydrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenylglyoxylic Acid | HCID 11915 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-(tert-butyl)benzohydrazide | HCID 1275961 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | N'-t-butyl-N'-benzoylcarbonyl-N-benzoylhydrazine | HCID 19368006 | 70% |
反応手順
N'-t-butyl-N'-benzoylhydrazine (1 g), benzoyl formic acid (0.7 g) and methanesulfonyl chloride (0.7 g) were stirred in toluene (30 ml) and saturated sodium bicarbonate (10 ml) at approximately 5° C. Triethylamine was added slowly, dropwise to the reaction mixture and stirred 1 hour at room temperature. After stirring for 1 hour, the reaction mixture was diluted with toluene (25 ml) and washed with water several times. The organic layers were dried over magnesium sulfate, filtered and the toluene rotavapped off to afford a white solid. After column chromatography, the product was obtained as a white solid in approximately 70% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424333 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-8c3ff157d51443f48a219a96f1d4bdcc |
| 出典メモ | uspto-grants-1995_06 |