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

HRID 258909노트

반응식

HRID 258909 반응식
[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

참가 물질

7

반응물 4

HCID 174Ethylene Glycol2회HCID 6101p-Toluenesulfonic acidHCID 10340Sodium CarbonateHCID 204801311-(3-Bromo-2-methylphenyl)ethanone

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aa07e73ca50745789165111f245b1659
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035376

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