Ethylene Glycol → 2-(3-Bromo-o-tolyl)-2-methyl-1,3-dioxolane

HRID 258909ノート

反応式

HRID 258909 の反応式
[Br:1][C:2]1[C:3](C)=[C:4]([C:8](=O)C)[CH:5]=[CH:6][CH:7]=1.[C:12]1(C)C=CC(S(O)(=O)=O)=C[CH:13]=1.[C:23](=[O:26])([O-])[O-:24].[Na+].[Na+].[CH2:29](O)CO>O.C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([C:23]2([CH3:29])[O:26][CH2:13][CH2:12][O:24]2)=[C:4]([CH3:8])[CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 174Ethylene Glycol2 回HCID 6101p-Toluenesulfonic acidHCID 10340Sodium CarbonateHCID 204801311-(3-Bromo-2-methylphenyl)ethanone

生成物 1

HCID 706381482-(3-Bromo-o-tolyl)-2-methyl-1,3-dioxolane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

A mixture of 100 parts of 3'-bromo-2'-methylacetophenone, 30 parts of ethylene glycol, 320 parts of anhydrous toluene and 2 parts of p-toluenesulfonic acid is stirred and refluxed for 4 hours with water-separator. A second fraction of 30 parts of ethylene glycol is added and stirring at reflux is continued for 18 hours. The reaction mixture is cooled and stirred for 30 minutes with 5 parts of sodium carbonate. The organic layer is separated, washed twice with water, dried and evaporated. The residue is distilled twice, yielding 2-(3-bromo-o-tolyl)-2-methyl-1,3-dioxolane; bp. 148°-150° C at 12 mm. pressure.

後処理

  1. stirringstirring
  2. temperatureat reflux
  3. temperatureThe reaction mixture is cooled
  4. customThe organic layer is separated
  5. washwashed twice with water
  6. customdried
  7. customevaporated
  8. distillationThe residue is distilled twice

出典と根拠

ORDレコード
ord-aa07e73ca50745789165111f245b1659
出典データセット
uspto-grants-1977_07
特許番号
US04035376

反応ノート

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