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

HRID 1010826
ノート
印刷プレビュー

反応式

HRID 1010826 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-d5c8c7c4799f47b9859592528f0666bc
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977342B2

反応ノート

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