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

HRID 462165
ノート
印刷プレビュー

反応式

HRID 462165 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8172Triethylene Glycol溶媒

反応条件

温度
175 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2a3e65bce37441c0b52621b428767dd9
出典データセット
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04065561

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート