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Ethylene Glycol → HCID 22281024、化合物

HRID 1062502
ノート
印刷プレビュー

反応式

HRID 1062502 の反応式
[CH:1]12[CH2:7][CH:4]([CH:5]=[CH:6]1)[CH2:3][CH:2]2[CH2:8][CH:9]=[O:10].[CH2:11](O)[CH2:12][OH:13].C1(C)C=CC=CC=1>C1(C)C=CC(S(O)(=O)=O)=CC=1.O>[CH:1]12[CH2:7][CH:4]([CH:5]=[CH:6]1)[CH2:3][CH:2]2[CH2:8][CH:9]1[O:13][CH2:12][CH2:11][O:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 174Ethylene GlycolHCID 1140TolueneHCID 5562742-(Bicyclo(2.2.1)hept-5-en-2-yl)acetaldehyde

生成物 1

HCID 22281024HCID 22281024、化合物収率 95%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 962Water溶媒

実験手順

40.0 g of (5-norbornen-2-yl)acetoaldehyde, 23.0 g of ethylene glycol, 120 ml of toluene and 200 mg of p-toluenesulfonic acid were mixed and heated under reflux for one hour while the water formed was removed through an H tube. The reaction mixture was allowed to cool down and poured into 50 ml of saturated sodium bicarbonate water. The resulting mixture separated into two layers. The organic layer was washed with water and saturated sodium chloride water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 50.3 g of 2-(5-norbornen-2-yl)methyl-1,3-dioxolane (boiling point 63° C./200 Pa, yield 95%).

後処理

  1. temperatureheated
  2. customformed
  3. customwas removed through an H tube
  4. temperatureto cool down
  5. additionpoured into 50 ml of saturated sodium bicarbonate water
  6. customThe resulting mixture separated into two layers
  7. washThe organic layer was washed with water and saturated sodium chloride water
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated in vacuum
  10. distillationIt was further purified by vacuum distillation

出典と根拠

ORDレコード
ord-4859b4df7e424d298f802ad34093c4e1
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06962767B2

反応ノート

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