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Hydrazine hydrate (1:1) → 1H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl-

HRID 465279
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반응식

HRID 465279 반응식
O.[NH2:2][NH2:3].[C:4]1(/[CH:10]=[CH:11]/[C:12](=O)[CH3:13])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CO>[CH3:13][C:12]1[CH2:11][CH:10]([C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[NH:3][N:2]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 637759Benzylideneacetone

생성물 1

HCID 101301011H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl-수율 74.8%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

17.1 g (342 mmol) of hydrazine monohydrate was dissolved in 500 ml of methanol. Then, 50 g (342 mmol) of trans-4-phenyl-3-buten-2-one dissolved in 100 ml of methanol was gradually dropwise added thereto under stirring within a range of from 5° C. to 15° C. Then, the mixture was stirred at room temperature for 30 hours, and methanol was distilled off under reduced pressure. The residue was distilled under reduced pressure to obtain 41.0 g of the desired 3-methyl-5-phenyl-2-pyrazoline.

후처리

  1. additionwas gradually dropwise added
  2. stirringThen, the mixture was stirred at room temperature for 30 hours
  3. distillationmethanol was distilled off under reduced pressure
  4. distillationThe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-e86188219a69483abe7df20cec0e3550
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05152824

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