Ethylene Glycol → 2-(2-Bromophenyl)-1,3-dioxolane

HRID 129586

反応式

HRID 129586 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[CH2:10](O)[CH2:11][OH:12]>C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]1[O:12][CH2:11][CH2:10][O:5]1

参加物

5

反応物 2

HCID 174Ethylene GlycolHCID 811292-Bromobenzaldehyde

生成物 1

HCID 5535342-(2-Bromophenyl)-1,3-dioxolane収率 98.6%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 1140Toluene溶媒

実験手順

A mixture of 2-bromobenzaldehyde (100 g; 0.54 mol), ethylene glycol (67.03 g; 1.08 mol), p-toluenesulphonic acid (0.5 g) and toluene was heated to and maintained at reflux temperature for 6 hours. During this period, water/ethylene glycol (23 ml) was removed by azeotropic distillation. The mixture was cooled and ether (1 l) was added. The ether solution was washed with saturated sodium bicarbonate solution (200 ml) water (3×150 ml) and saturated brine (1×150 ml). After drying and filtration, evaporation of the ether solution gave 2-(2-bromophenyl)-1,3-dioxolane (121.96 g, 98.6% yield) as an oil.

後処理

  1. temperaturewas heated to and
  2. temperaturemaintained
  3. temperatureat reflux temperature for 6 hours
  4. waitDuring this period
  5. customwater/ethylene glycol (23 ml) was removed by azeotropic distillation
  6. temperatureThe mixture was cooled
  7. additionether (1 l) was added
  8. washThe ether solution was washed with saturated sodium bicarbonate solution (200 ml) water (3×150 ml) and saturated brine (1×150 ml)
  9. customAfter drying
  10. filtrationfiltration, evaporation of the ether solution

出典と根拠

ORDレコード
ord-df3d23cae80f4fa2a29f02eb22d0e312
出典データセット
uspto-grants-1995_11
特許番号
US05468857

関連ノート

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