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Propanoic acid, 2-bromo-2-methyl-, ethyl ester → HCID 14871449、化合物

HRID 2058076
ノート
印刷プレビュー

反応式

HRID 2058076 の反応式
[Na].[C:2]1([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:18]([CH3:25])([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(O)C>[C:2]1([N:8]=[CH:9][C:10]2[CH:11]=[CH:12][C:13]([O:16][C:18]([CH3:25])([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:14][CH:15]=2)[CH:3]=[CH:4][CH:5]=[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 74319Phenol, 4-[(phenylimino)methyl]-HCID 5360545Sodium

生成物 1

HCID 14871449HCID 14871449、化合物収率 69.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(a) To 170 ml of absolute ethanol is added 1.48 g of sodium, and 8.4 g of 4-(N-phenylformimidoyl)phenol is added to the mixture at room temperature with stirring to prepare a solution. 12.5 g of ethyl 2-bromo-2-methylpropionate is added to the solution, and the mixture is refluxed under heating for 5 hours. After the reaction, the ethanol is distilled off. The residue is dissolved in ether and thereafter washed with 5% aqueous solution of sodium hydroxide and then with water. After drying the resulting mixture, the ether is distilled off to give 9.2 g of ethyl 2-[4-(N-phenylformimidoyl)phenoxy]-2-methylpropionate. Infrared absorption spectrum (liquid film) 1735, 1280, 1245, 1170, 1140, 1020 cm-1.

後処理

  1. additionis added to the mixture at room temperature
  2. customto prepare a solution
  3. temperaturethe mixture is refluxed
  4. temperatureunder heating for 5 hours
  5. customAfter the reaction
  6. distillationthe ethanol is distilled off
  7. dissolutionThe residue is dissolved in ether
  8. washwashed with 5% aqueous solution of sodium hydroxide
  9. customAfter drying the resulting mixture
  10. distillationthe ether is distilled off

出典と根拠

ORDレコード
ord-94096d4f017542c5ad3607851d68072a
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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