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Propanoic acid, 2-bromo-2-methyl-, ethyl ester → HCID 20329874、化合物

HRID 2058083
ノート
印刷プレビュー

反応式

HRID 2058083 の反応式
[Na].[C:2]1([CH3:17])[CH:7]=[CH:6][C:5]([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.Br[C:19]([CH3:26])([CH3:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21]>C(O)C>[C:2]1([CH3:17])[CH:3]=[CH:4][C:5]([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:19]([CH3:26])([CH3:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21])=[CH:12][CH:11]=2)=[CH:6][CH:7]=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 6111664-{(E)-[(4-methylphenyl)imino]methyl}phenolHCID 5360545Sodium

生成物 1

HCID 20329874HCID 20329874、化合物収率 61.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(a) To 50 ml of absolute ethanol is added 0.58 g of sodium, and 4.2 g of 4-[N-(p-tolyl)formimidoyl]phenol and then 7.84 g of ethyl 2-bromo-2-methylpropionate are added to the solution at room temperature with stirring. The mixture is refluxed under heating and with stirring for 5 hours on an oil bath. After distilling off the ethanol from the reaction mixture, the residue is dissolved in ether. The solution is washed with 5% aqueous solution of sodium hydroxide and then with water. After drying the solution, the ether is distilled off, and the residue is further concentrated under reduced pressure on an oil bath at 100° C. to give 4.0 g of ethyl 2-[4-{N-(p-tolyl)formimidoyl}phenoxy]-2-methylpropionate as an oily product.

後処理

  1. temperatureThe mixture is refluxed
  2. temperatureunder heating
  3. stirringwith stirring for 5 hours on an oil bath
  4. distillationAfter distilling off the ethanol from the reaction mixture
  5. dissolutionthe residue is dissolved in ether
  6. washThe solution is washed with 5% aqueous solution of sodium hydroxide
  7. customAfter drying the solution
  8. distillationthe ether is distilled off
  9. concentrationthe residue is further concentrated under reduced pressure on an oil bath at 100° C.

出典と根拠

ORDレコード
ord-67ed7e337b5847bba5f361e2a1d148d5
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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