Triethylamine → 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde

HRID 2283187ノート

反応式

HRID 2283187 の反応式
C(N(CC)CC)C.Cl[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH:15]([F:17])[F:16])[C:10]=1[CH:18]=[O:19]>C(O)C.[Pd]>[CH3:14][N:13]1[CH:9]=[C:10]([CH:18]=[O:19])[C:11]([CH:15]([F:16])[F:17])=[N:12]1

参加物

5

反応物 2

HCID 8471TriethylamineHCID 197546925-Chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde

生成物 1

HCID 533020643-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde収率 89.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

反応条件

温度
30 °C

実験手順

In an autoclave, 10 g of 5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde were dissolved in 150 ml of ethanol, and 10.4 g of triethylamine and 500 mg of 5% palladium on calcium carbonate were added. The autoclave was flushed with nitrogen and subsequently pressurised to 5 bar hydrogen. The reaction mixture was then stirred at 30° C. for 4 h. After filtration of the catalyst, the solvent was removed under reduced pressure and the product was obtained as a solid (7.4 g) having a melting point of 46-47° C.

後処理

  1. customThe autoclave was flushed with nitrogen
  2. filtrationAfter filtration of the catalyst
  3. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-1fd79fa2c380483389fd7c208331b22d
出典データセット
uspto-grants-2015_09
特許番号
US09145369B2

反応ノート

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