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Water → HCID 10160441, 화합물

HRID 1759692
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HRID 1759692 반응식
Cl[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:9][N:8]=2)[N:5]=[C:4]([C:17]([F:20])([F:19])[F:18])[C:3]=1[C:21]#[N:22].[CH2:23]=[C:24]1[CH2:29][CH2:28][CH:27]([CH2:30][OH:31])[CH2:26][CH2:25]1.[F-].[K+].O>CS(C)=O>[CH3:16][S:13]([C:10]1[CH:11]=[CH:12][C:7]([N:6]2[C:2]([O:31][CH2:30][CH:27]3[CH2:28][CH2:29][C:24](=[CH2:23])[CH2:25][CH2:26]3)=[C:3]([C:21]#[N:22])[C:4]([C:17]([F:20])([F:19])[F:18])=[N:5]2)=[N:8][CH:9]=1)(=[O:15])=[O:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 962WaterHCID 138604-MethylenecyclohexylmethanolHCID 522689Potassium FluorideHCID 12135150HCID 12135150, 화합물

생성물 1

HCID 10160441HCID 10160441, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

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온도
20 °C

실험 절차

5-Chloro-1-(5-methanesulfonyl-pyridin-2-yl)-3-trifluoromethyl-1H-pyrazole-4-carbonitrile (351 mg, 1 mmol) and (4-methylene-cyclohexyl)-methanol (252 mg, 2 mmol) were dissolved in dry dimethylsulfoxide (DMSO) (5 ml) and potassium fluoride (116 mg, 2 mmol) was added to the DMSO solution. The resulting mixture was stirred at 20° C. for a period of 48 hours. Analytical HPLC indicated the reaction completion. The reaction mixture was poured into water (15 ml) and the resulting mixture was extracted with ethyl acetate (20 ml). The organic extract was dried over magnesium sulfate and concentrated with a rotary evaporator. The desired product was isolated by chromatography on silica gel column. MS: 441, r.t.: 3.0 min.

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate (20 ml)
  2. extractionThe organic extract
  3. dry with materialwas dried over magnesium sulfate
  4. concentrationconcentrated with a rotary evaporator

출처 및 근거

ORD 기록
ord-b1823c8cf07e4b5eb837f60bcbf0557d
출처 데이터셋
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06838458B2

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