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Triethylamine → 2-[2-(Benzyloxy)ethoxy]ethyl acrylate

HRID 926822
ノート
印刷プレビュー

反応式

HRID 926822 の反応式
[CH2:1]([O:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][OH:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:22](Cl)(=[O:25])[CH:23]=[CH2:24]>C1COCC1>[C:22]([O:14][CH2:13][CH2:12][O:11][CH2:10][CH2:9][O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)(=[O:25])[CH:23]=[CH2:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 2297222-[2-(Benzyloxy)ethoxy]ethan-1-ol

生成物 1

HCID 667019012-[2-(Benzyloxy)ethoxy]ethyl acrylate収率 84%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a 1 L three-neck round bottom flask equipped with mechanical stirrer were charged diethylene glycol monobenzyl ether (98.0 g, 0.5 mol), anhydrous triethylamine (120 mL, 0.85 mol), and anhydrous THF (300 mL). The solution was cooled in an ice/salt bath under dry air blanket for 15 minutes. Acryloyl chloride (55 mL, 0.68 mol) was added into the vigorously stirred cold solution through an addition funnel over 90 minutes and the addition rate was adjusted to keep the temperature of the reaction mixture below 10° C. After the addition, the reaction mixture was stirred in the ice/salt bath for additional two hours followed by quenching with the addition of 2M HCl (400 mL). The mixture was extracted with ethyl acetate (300 mL×3) and the combined organic layer was washed with DI water (200 mL×3), aqueous sodium bicarbonate (200 mL×2), and dried over MgSO4. Filtration and removal of solvents under reduced pressure gave the crude product as light brown oil which was purified on silica gel using Hexanes/Ethyl acetate (4/1, v/v) as eluent to give the final product as a colorless oil (105.0 g, 0.42 mol, yield: 84%).

後処理

  1. customTo a 1 L three-neck round bottom flask equipped with mechanical stirrer
  2. temperatureThe solution was cooled in an ice/salt bath
  3. customunder dry air blanket for 15 minutes
  4. customthe temperature of the reaction mixture below 10° C
  5. additionAfter the addition
  6. customby quenching with the addition of 2M HCl (400 mL)
  7. extractionThe mixture was extracted with ethyl acetate (300 mL×3)
  8. washthe combined organic layer was washed with DI water (200 mL×3), aqueous sodium bicarbonate (200 mL×2)
  9. dry with materialdried over MgSO4
  10. filtrationFiltration and removal of solvents under reduced pressure
  11. customgave the crude product as light brown oil which
  12. customwas purified on silica gel

出典と根拠

ORDレコード
ord-ca149ce7404d4030a736631683f787fd
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09289531B2

反応ノート

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