참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | 1-Propanone, 1-(4-chlorophenyl)-3-(dimethylamino)-, hydrochloride (1:1) | HCID 200370 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3-(4-Chlorophenyl)-4,5-dihydro-1H-pyrazole | HCID 13143700 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08722887B2 |
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| 출처 데이터셋 | uspto-grants-2014_05 |
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| ORD ID | ord-92c5b61e2c3a4d50b6f5137860c46781 |
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| 출처 메모 | uspto-grants-2014_05 |
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