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Ethylene Glycol → HCID 22281024, 화합물

HRID 1058154
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HRID 1058154 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 22281024HCID 22281024, 화합물수율 95%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-4ee75d8673e74a8db963b4ae9bbba8cf
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06515149B2

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