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2-Fluorobenzoyl chloride → N-(4-Cyano-1,3-dimethyl-1H-pyrazol-5-yl)-2-fluorobenzamide

HRID 1010826
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HRID 1010826 반응식
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([CH3:8])[C:3]=1[C:9]#[N:10].[F:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14](Cl)=[O:15]>N1C=CC=CC=1>[C:9]([C:3]1[C:4]([CH3:8])=[N:5][N:6]([CH3:7])[C:2]=1[NH:1][C:14](=[O:15])[C:13]1[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=1[F:11])#[N:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 98082-Fluorobenzoyl chlorideHCID 2198705-amino-1,3-dimethyl-1H-pyrazole-4-carbonitrile

생성물 1

HCID 17088883N-(4-Cyano-1,3-dimethyl-1H-pyrazol-5-yl)-2-fluorobenzamide수율 50%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

5-Amino-1,3-dimethyl-1H-pyrazole-4-carbonitrile (10 g, 73.4 mmole) was suspended in pyridine (90 ml) and 2-fluorobenzoyl chloride was added dropwise while cooling the reaction mixture on an ice bath. The mixture reaction was stirred overnight at room temperature. Most of the pyridine was removed and 100 ml of cold water was added to precipitate the product. The product was isolated by filtration, washed with cold water and a small amount of cold ethanol, and dried under vacuum to obtain 9.15 g of product (yield: 50%).

후처리

  1. temperaturewhile cooling the reaction mixture on an ice bath
  2. customThe mixture reaction
  3. customMost of the pyridine was removed
  4. addition100 ml of cold water was added
  5. customto precipitate the product
  6. customThe product was isolated by filtration
  7. washwashed with cold water
  8. dry with materiala small amount of cold ethanol, and dried under vacuum

출처 및 근거

ORD 기록
ord-d5c8c7c4799f47b9859592528f0666bc
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977342B2

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