関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 1-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1) | HCID 92844 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Phenyl-4,5-dihydro-1H-pyrazole | HCID 589745 | — |
反応手順
Under N2 atmosphere, 3-dimethylamino-1-phenyl-propan-1-one hydrochloride (37.2 g) was dissolved in warm MeOH (75 mL), and slowly added to a solution of hydrazine hydrate (23 mL) and 50% aqueous NaOH (12 mL) in MeOH (30 mL) stirred at 50° C. The mixture was refluxed for 2 hours and evaporated under reduced pressure. Ice water was added to the residue and after stirring for 5 minutes the formed solid was filtered off. The residue was taken up in Et2O, dried over Na2SO4, and evaporated to dryness under reduced pressure to give 19.7 g of a yellow oil being 80% pure, which was used in subsequent steps without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08722887B2 |
|---|
| 出典データセット | uspto-grants-2014_05 |
|---|
| ORD ID | ord-0b6130dbe17e45fe952bddcd87bdcf0e |
|---|
| 出典メモ | uspto-grants-2014_05 |
|---|
