Ethylene Glycol → HCID 22281032、化合物

HRID 1058156ノート

反応式

HRID 1058156 の反応式
[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

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 69733599HCID 69733599、化合物HCID 86585896Sodium bicarbonate water

生成物 1

HCID 22281032HCID 22281032、化合物収率 85%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6565c6debb194bdaaffe392505f666aa
出典データセット
uspto-grants-2003_02
特許番号
US06515149B2

反応ノート

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