Dimethylformamide → 5-Chloro-1-ethyl-3-methyl-1H-pyrazole-4-carbaldehyde

HRID 47629ノート

反応式

HRID 47629 の反応式
CN(C)[CH:3]=[O:4].P(Cl)(Cl)([Cl:8])=O.[CH2:11]([N:13]1[C:17](O)=[CH:16][C:15]([CH3:19])=[N:14]1)[CH3:12]>O>[Cl:8][C:17]1[N:13]([CH2:11][CH3:12])[N:14]=[C:15]([CH3:19])[C:16]=1[CH:3]=[O:4]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 178463089HCID 178463089、化合物

生成物 1

HCID 227475065-Chloro-1-ethyl-3-methyl-1H-pyrazole-4-carbaldehyde

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To 28.7 ml of anhydrous N,N-dimethylformamide at 0° C. were added slowly 80.7 ml of phosphorus oxychloride then 15.6 g of 2-ethyl-5-methyl-2H-pyrazol-3-ol. The mixture was stirred under nitrogen at 80° C. for 1 hour, poured into 700 ml of water at 0° C. then extracted six times with 350 ml of diethyl ether. The combined extracts were dried over magnesium sulphate, filtered and evaporated to leave 9.3 g of 5-chloro-1-ethyl-3-methyl-1H-pyrazole-4-carbaldehyde as an orange liquid which was used without further purification.

後処理

  1. extractionthen extracted six times with 350 ml of diethyl ether
  2. dry with materialThe combined extracts were dried over magnesium sulphate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-bbcc7bc887b045c394ac64c27e654894
出典データセット
uspto-grants-2004_03
特許番号
US06699887B2

反応ノート

読み込み中…