4-Toluenesulfonyl chloride → Ethyl 2-(4-vinylphenoxy)isobutyrate

HRID 1605119ノート

反応式

HRID 1605119 の反応式
O[CH:2]([C:4]1[CH:18]=[CH:17][C:7]([O:8][C:9]([CH3:16])([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:6][CH:5]=1)[CH3:3].C1(C)C=CC(S(Cl)(=O)=O)=CC=1>N1C=CC=CC=1>[CH:2]([C:4]1[CH:18]=[CH:17][C:7]([O:8][C:9]([CH3:16])([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:6][CH:5]=1)=[CH2:3]

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 103599Ethyl 2-(4-(1-hydroxyethyl)phenoxy)isobutyrate

生成物 1

HCID 104107Ethyl 2-(4-vinylphenoxy)isobutyrate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 116 g. of ethyl 2-[4-(1-hydroxyethyl)phenoxy]-2-methylpropionate and 92 g. of p-toluenesulfonyl chloride in 500 ml. of pyridine was heated at reflux for three hours, kept at room temperature for about 16 hours and then heated at reflux again for six hours. The reaction mixture was poured into ice water and extracted with hexane. The hexane solution was washed successively with dilute sulfuric acid, 10% potassium bicarbonate, water and saturated sodium chloride solution, then dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was distilled at 104°-111°C. (0.03-0.08 mm.) to give60 g. of ethyl 2-(p-vinylphenoxy)-2-methylpropionate.

後処理

  1. additionA mixture of 116 g
  2. temperatureat reflux for three hours
  3. temperatureheated
  4. temperatureat reflux again for six hours
  5. extractionextracted with hexane
  6. washThe hexane solution was washed successively with dilute sulfuric acid, 10% potassium bicarbonate, water and saturated sodium chloride solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. distillationThe residue was distilled at 104°-111°C. (0.03-0.08 mm.) to give60

出典と根拠

ORDレコード
ord-9d0e138a466847e68b01e9ff93c5274b
出典データセット
uspto-grants-1976_04
特許番号
US03948973

反応ノート

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