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Propanoic acid, 2-bromo-2-methyl-, ethyl ester → HCID 20329847、化合物

HRID 2058080
ノート
印刷プレビュー

反応式

HRID 2058080 の反応式
[Na].[CH:2]1([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.Br[C:18]([CH3:25])([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(O)C>[CH:2]1([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:18]([CH3:25])([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:12][CH:11]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1
参加物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 11745Propanoic acid, 2-bromo-2-methyl-, ethyl esterHCID 2412384-[(Cyclohexylimino)methyl]phenolHCID 5360545Sodium

生成物 1

HCID 20329847HCID 20329847、化合物収率 50.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(a) To 70 ml of absolute ethanol is added 872 mg of sodium, and 7 g of 4-(N-cyclohexylformimidoyl)phenol is added to the solution. Subsequently, 7.4 g of ethyl 2-bromo-2-methylpropionate is further added. The mixture is refluxed under heating and with stirring for 15 hours. After distilling off the ethanol from the reaction mixture, water is added to the residue, and the solution is extracted three times with benzene. The extract is washed with water twice, with cooled dilute aqueous solution of sodium hydroxide three times and then with water twice. After drying the resulting solution over magnesium sulfate, the solvent is distilled off to give 5.54 g of ethyl 2-[4-(N-cyclohexylformimidoyl)phenoxy]-2-methylpropionate as an oil.

後処理

  1. additionis added to the solution
  2. temperatureThe mixture is refluxed
  3. temperatureunder heating
  4. distillationAfter distilling off the ethanol from the reaction mixture, water
  5. additionis added to the residue
  6. extractionthe solution is extracted three times with benzene
  7. washThe extract is washed with water twice
  8. temperaturewith cooled dilute aqueous solution of sodium hydroxide three times
  9. dry with materialAfter drying the resulting solution over magnesium sulfate
  10. distillationthe solvent is distilled off

出典と根拠

ORDレコード
ord-ab3ae68d7a6e40e59afeed458ea3b612
出典データセット
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04214094

反応ノート

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