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Ammonium hydroxide methanol → HCID 66958288, 화합물

HRID 1360456
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HRID 1360456 반응식
[CH2:1]([C:3]1[N:7]([CH2:8][CH2:9][CH3:10])[N:6]=[C:5]([C:11]([O:13]CC)=O)[CH:4]=1)[CH3:2].[OH-].[NH4+:17].CO>>[CH2:1]([C:3]1[N:7]([CH2:8][CH2:9][CH3:10])[N:6]=[C:5]([C:11]([NH2:17])=[O:13])[CH:4]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 21894508Ammonium hydroxide methanolHCID 66958661HCID 66958661, 화합물

생성물 1

HCID 66958288HCID 66958288, 화합물

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온도
125 °C

실험 절차

Ethyl 5-ethyl-1-propyl-1H-pyrazole-3-carboxylate (13.0 g, 62 mmol) in a 4:1 mixture of concentrated ammonium hydroxide/methanol (50 mL) was heated at 125° C. for 18 hours in a pressure vessel. After cooling to ambient temperature, the contents of the vessel were poured into a flask and a precipitate formed immediately. The precipitate was isolated by filtration to yield 5.02 g of analytically pure 5-ethyl-1-propyl-1H-pyrazole-3-carboxamide as off-white crystals, mp 105-106° C. MS (APCI) m/z 182.1 (M+H)+; Anal. calcd for C9H15N3O: C, 59.64; H, 8.34; N, 23.19. Found: C, 59.59; H, 8.54; N, 23.39. An additional 0.50 g of product was obtained in the second crop from the filtrate.

후처리

temperature
After cooling to ambient temperature
  • additionthe contents of the vessel were poured into a flask
  • customa precipitate formed immediately
  • customThe precipitate was isolated by filtration
  • 출처 및 근거

    ORD 기록
    ord-fbb789797caa4142b5d4a0a87ca8dd16
    출처 데이터셋
    uspto-grants-2011_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07879849B2

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