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, 1-(4-chlorophenyl)-3-(dimethylamino)-, hydrochloride (1:1) | HCID 200370 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(4-Chlorophenyl)-4,5-dihydro-1H-pyrazole | HCID 13143700 | — |
反応手順
Under N2 atmosphere, 1-(4-chloro-phenyl)-3-dimethylamino-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. Water was added to the residue, followed by extraction with DCM. The organic phase was washed twice with water, dried and evaporated under reduced pressure, to give 25.0 g of a yellow solid, m.p. 90-100° C.
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-92c5b61e2c3a4d50b6f5137860c46781 |
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| 出典メモ | uspto-grants-2014_05 |
|---|
