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HCID 19361727、化合物 → 6-(Dimethylamino)pyridine-2-carbaldehyde

HRID 376276
ノート
印刷プレビュー

反応式

HRID 376276 の反応式
[O:1]1CCO[CH:2]1[C:6]1[N:11]=[C:10]([N:12]([CH3:14])[CH3:13])[CH:9]=[CH:8][CH:7]=1>C(O)=O>[CH3:13][N:12]([CH3:14])[C:10]1[N:11]=[C:6]([CH:2]=[O:1])[CH:7]=[CH:8][CH:9]=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

3

反応物 1

HCID 19361727HCID 19361727、化合物

生成物 1

HCID 158584806-(Dimethylamino)pyridine-2-carbaldehyde

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
60 °C

実験手順

0.60 g of (6-[1,3]dioxolan-2-yl-pyridin-2-yl)dimethylamine (3.09 mmol) is mixed in 10 ml of an aqueous solution of formic acid at 80% and then the solution is heated at 60° C. for 20 hours. The solvents are removed by azeotropic entrainment with toluene, the residue is taken up in water, the mixture is cooled to 0° C. and then the medium is basified by addition of potassium carbonate. The mixture is extracted with ethyl acetate, the organic phase is washed with water and then with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, filtered, and the solvent is evaporated under vacuum. The title product is obtained in the form of a yellow oil (0.43 g) which is used in the next stage without further purification.

後処理

  1. customThe solvents are removed by azeotropic entrainment with toluene
  2. temperaturethe mixture is cooled to 0° C.
  3. additionthe medium is basified by addition of potassium carbonate
  4. extractionThe mixture is extracted with ethyl acetate
  5. washthe organic phase is washed with water
  6. dry with materialwith a saturated aqueous solution of sodium chloride, dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent is evaporated under vacuum

出典と根拠

ORDレコード
ord-edd6a7625ae64fe2b2419730173bbda0
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06020345

反応ノート

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