참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | 1-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1) | HCID 92844 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3-Phenyl-4,5-dihydro-1H-pyrazole | HCID 589745 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07728018B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-97522613bb9a4da1bcaf9856395657d5 |
|---|
| 출처 메모 | uspto-grants-2010_06 |
|---|
