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Potassium Hydroxide → 3-(1,5-Dimethyl-1H-pyrrol-2-yl)pyridine

HRID 462165
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HRID 462165 반응식
[CH3:1][N:2]1[C:6]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[CH:5][CH:4]=[C:3]1[CH:13]=O.O.NN.[OH-].[K+]>C(O)COCCOCCO>[CH3:1][N:2]1[C:3]([CH3:13])=[CH:4][CH:5]=[C:6]1[C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1
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참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 213906921-Methyl-5-(pyridin-3-yl)-1H-pyrrole-2-carbaldehyde

생성물 1

HCID 536472703-(1,5-Dimethyl-1H-pyrrol-2-yl)pyridine

시약·촉매·용매 1

HCID 8172Triethylene Glycol용매

반응 조건

온도
175 °C

실험 절차

A mixture of 1-methyl-5-(3-pyridyl) pyrrole-2-carboxaldehyde (8.0 g, 43 mmoles), hydrazine hydrate (8.0 g, 160 mmoles) and potassium hydroxide (10.6 g of 85% pellets) in 80 ml triethyleneglycol is stirred at 125° L C for 75 min. during which time vigorous evolution of gas is observed. The temperature is then increased to 175° C and stirring continued until evolution of gas ceases. After cooling, the reaction mixture is extracted with 3 × 50 ml portions of diethyl ether. The combined ether layers are dried (anhydrous magnesium sulfate) and removed under vacuum. Fractional vacuum distillation of the residue provides the pure product.

후처리

  1. stirringstirring
  2. temperatureAfter cooling
  3. extractionthe reaction mixture is extracted with 3 × 50 ml portions of diethyl ether
  4. dry with materialThe combined ether layers are dried (anhydrous magnesium sulfate)
  5. customremoved under vacuum
  6. distillationFractional vacuum distillation of the residue
  7. customprovides the pure product

출처 및 근거

ORD 기록
ord-2a3e65bce37441c0b52621b428767dd9
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04065561

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