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

HRID 1354295
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HRID 1354295 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 reaction mixture on an ice bath. Stirred reaction mixture overnight at room temperature. Removed most of the pyridine and added 100 ml cold water to precipitate the product. Isolated product by filtration, washed with cold water, small amount of cold ethanol and dried under vacuum to obtain 9.15 g product (yield: 50%).

후처리

  1. temperaturewhile cooling
  2. customreaction mixture on an ice bath
  3. customreaction mixture overnight at room temperature
  4. customRemoved most of the pyridine
  5. additionadded 100 ml cold water
  6. customto precipitate the product
  7. filtrationIsolated product by filtration
  8. washwashed with cold water, small amount of cold ethanol
  9. customdried under vacuum

출처 및 근거

ORD 기록
ord-d2f4b17e7a6d4c1b8ac44150bdc5681c
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223766B2

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