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

HRID 47629노트

반응식

HRID 47629 반응식
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]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 178463089HCID 178463089, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bbcc7bc887b045c394ac64c27e654894
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699887B2

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