Ethylene Glycol → HCID 22281032, 화합물

HRID 1058156노트

반응식

HRID 1058156 반응식
[CH2:1]([O:3][CH:4]=[CH:5][CH2:6][CH2:7][CH:8]1[CH2:13][CH:12]2[CH2:14][CH:9]1[CH:10]=[CH:11]2)[CH3:2].C(O)C[OH:17].C1(C)C=CC(S(O)(=O)=O)=CC=1.O.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[CH:9]12[CH2:14][CH:12]([CH:11]=[CH:10]1)[CH2:13][CH:8]2[CH2:7][CH2:6][CH2:5][CH:4]1[O:17][CH2:2][CH2:1][O:3]1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 69733599HCID 69733599, 화합물HCID 86585896Sodium bicarbonate water

생성물 1

HCID 22281032HCID 22281032, 화합물수율 85%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Next, the thus obtained 5-(4-ethoxy-3-buten-1-yl)-2-norbornene was mixed with 90 g of ethylene glycol, 1.0 g of p-toluenesulfonic acid and 300 ml of toluene and heated under reflux for one hour. The reaction mixture was allowed to cool down and poured into 100 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 177 g of 2-{3-(5-norbornen-2-yl)-1-propyl}-1,3-dioxolane (boiling point 92° C./27 Pa, yield 85%).

후처리

  1. temperatureheated
  2. temperatureunder reflux for one hour
  3. temperatureto cool down
  4. customThe resulting mixture separated into two layers
  5. washThe organic layer was washed with water and saturated sodium chloride water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuum
  8. distillationIt was further purified by vacuum distillation

출처 및 근거

ORD 기록
ord-6565c6debb194bdaaffe392505f666aa
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06515149B2

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