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Ethanol → HCID 70817737, 화합물

HRID 82228
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HRID 82228 반응식
[OH-:1].[Na+].[CH:3]([N:6]1[C:10]([C:11]([F:14])([F:13])[F:12])=[C:9](CC#N)[CH:8]=[N:7]1)([CH3:5])[CH3:4].[CH3:18][CH2:19][OH:20]>>[CH:3]([N:6]1[C:10]([C:11]([F:14])([F:13])[F:12])=[C:9]([CH2:18][C:19]([OH:1])=[O:20])[CH:8]=[N:7]1)([CH3:5])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 70817665HCID 70817665, 화합물

생성물 1

HCID 70817737HCID 70817737, 화합물수율 75%

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온도
60 °C

실험 절차

Aqueous sodium hydroxide (150 mL of a 1 M solution) was added to [1-isopropyl-5-(trifluoromethyl)-1H-pyrazol-4-yl]acetonitrile (Preparation 184, 6.2 g, 28.6 mmol) in EtOH (150 mL) and the mixture was heated at 60° C. for 16 hours. The mixture was evaporated in vacuo and the residue was dissolved in water (50 mL) then washed with EtOAc (100 mL). The aqueous phase was acidified to pH 5 using 1N HCl and extracted with 10% IPA in DCM (4×100 mL). The combined organic phases were dried over sodium sulphate and evaporated in vacuo to afford the title compound as a white solid in 75% yield, 5.0 g.

후처리

  1. customThe mixture was evaporated in vacuo
  2. dissolutionthe residue was dissolved in water (50 mL)
  3. washthen washed with EtOAc (100 mL)
  4. extractionextracted with 10% IPA in DCM (4×100 mL)
  5. dry with materialThe combined organic phases were dried over sodium sulphate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-2ca0929cdc1943a5bb7da6b308a0cd5c
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846698B2

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