Hydrochloric Acid → 1-(1,3-dimethyl-1H-pyrazol-4-yl)ethan-1-one

HRID 62220노트

반응식

HRID 62220 반응식
[CH3:1][N:2]([CH:7]=[C:8]([C:12](=[O:14])[CH3:13])[C:9](=O)[CH3:10])[N:3]=C(C)C.Cl>C(O)C.O>[CH3:1][N:2]1[CH:7]=[C:8]([C:12](=[O:14])[CH3:13])[C:9]([CH3:10])=[N:3]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 236352723-((1-Methyl-2-(propan-2-ylidene)hydrazinyl)methylene)pentane-2,4-dione

생성물 1

HCID 8439771-(1,3-dimethyl-1H-pyrazol-4-yl)ethan-1-one

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

3-((1-methyl-2-(propan-2-ylidene)hydrazinyl)methylene)pentane-2,4-dione (Preparation 3, 9.1 g) was dissolved in Ethanol (20 mL) and treated with 1M Hydrogen chloride in Water (20 mL), the reaction solution was stirred at room temperature for 15 minutes. The reaction solution was then concentrated under vacuum with a rotavap to approximately 20 mL total volume. The reaction solution was then treated with saturated aqueous sodium bicarbonate (45 mL), and extracted with methylene chloride (4×50 mL) The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo afford the title compound as a light orange solid. (6.2 g, 97%).

후처리

  1. concentrationThe reaction solution was then concentrated under vacuum with a rotavap to approximately 20 mL total volume
  2. additionThe reaction solution was then treated with saturated aqueous sodium bicarbonate (45 mL)
  3. extractionextracted with methylene chloride (4×50 mL) The combined organic extracts
  4. dry with materialwere dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-985c132fa4894d0b82cf4737d412a941
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09446046B2

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