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Sodium Hydroxide → HCID 86692504, 화합물

HRID 1748557
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HRID 1748557 반응식
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:12]2[C:17]([F:18])=[CH:16][C:15]([C:19]([F:22])([F:21])[F:20])=[CH:14][N:13]=2)[C:10]=1[CH3:11])=[O:5])C.[OH-].[Na+]>O1CCCC1>[F:18][C:17]1[C:12]([N:9]2[C:10]([CH3:11])=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]2)=[N:13][CH:14]=[C:15]([C:19]([F:22])([F:20])[F:21])[CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 86692473HCID 86692473, 화합물

생성물 1

HCID 86692504HCID 86692504, 화합물수율 85.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-[3-fluoro-5-(trifluoromethyl)pyridin-2-yl]-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (2.17 g) in tetrahydrofuran (10 ml) was added 1 N aqueous solution of sodium hydroxide (10 ml), and stirred at room temperature overnight. After completion of the reaction, the organic solvent was evaporated in vacuo, then water and diethyl ether were added thereto, and the aqueous layer was separated. To the aqueous layer was added 1 N hydrochloric acid aqueous solution under ice-cooling to adjust the layer to pH 5, the precipitated solid was collected by filtration, and dried at 60° C. under air blow to give the titled compound (1.7 g) as a white solid. MS (ESI) m/z: 290 (M+H)+.

후처리

  1. customAfter completion of the reaction
  2. customthe organic solvent was evaporated in vacuo
  3. additionwater and diethyl ether were added
  4. customthe aqueous layer was separated
  5. additionTo the aqueous layer was added 1 N hydrochloric acid aqueous solution under ice-
  6. temperaturecooling
  7. filtrationthe precipitated solid was collected by filtration
  8. customdried at 60° C. under air blow

출처 및 근거

ORD 기록
ord-70cdd2f853f5418180de7090c7877b95
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150555B2

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