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Methanol → HCID 86692472, 화합물

HRID 1748524
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HRID 1748524 반응식
[OH-:1].[Na+].O.C([O:6][C:7]([C:9]1[CH:10]=[N:11][N:12]([C:15]2[C:20](F)=[CH:19][C:18]([C:22]([F:25])([F:24])[F:23])=[CH:17][N:16]=2)[C:13]=1[CH3:14])=[O:8])C.[CH3:26]O>O1CCCC1>[CH3:26][O:1][C:20]1[C:15]([N:12]2[C:13]([CH3:14])=[C:9]([C:7]([OH:6])=[O:8])[CH:10]=[N:11]2)=[N:16][CH:17]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 14798Sodium HydroxideHCID 86692473HCID 86692473, 화합물

생성물 1

HCID 86692472HCID 86692472, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4N Aqueous solution of sodium hydroxide (20 ml) and water (20 ml) were added to a solution of 1-[3-fluoro-5-(trifluromethyl)pyridin-2-yl]-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (3 g) in methanol (20 ml) and tetrahydrofuran (20 ml), and stirred at room temperature for five hours. After completion of the reaction, the organic solvent was evaporated, diethylether and water was added to the residue. The aqueous layer was separated, pH was adjusted to 5 by the addition of concentrated hydrochloric acid under ice cooling, and the precipitated solid was collected by filtration dried at 60° C. under air blow to give the titled compound (1.17 g) as a white solid.

후처리

  1. customAfter completion of the reaction
  2. customthe organic solvent was evaporated
  3. additiondiethylether and water was added to the residue
  4. customThe aqueous layer was separated
  5. additionpH was adjusted to 5 by the addition of concentrated hydrochloric acid under ice cooling
  6. filtrationthe precipitated solid was collected by filtration
  7. customdried at 60° C. under air blow

출처 및 근거

ORD 기록
ord-1a7dfa76143b42e49c9e21b3c8f67bd6
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150555B2

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