Ethylene Glycol → 2-Ethyl-2-2-thienyl-[1,3]dioxolane

HRID 49326ノート

反応式

HRID 49326 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6](=[O:9])[CH2:7][CH3:8].C[Si](Cl)(C)C.[CH2:15](O)[CH2:16][OH:17]>>[CH2:7]([C:6]1([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)[O:17][CH2:16][CH2:15][O:9]1)[CH3:8]

参加物

4

反応物 3

HCID 174Ethylene GlycolHCID 6397ChlorotrimethylsilaneHCID 261792-Propionylthiophene

生成物 1

HCID 179347502-Ethyl-2-2-thienyl-[1,3]dioxolane

実験手順

30 g (214.3 mmol) of 1-2-thienyl-1-propanone are dissolved in 120 mL of ethylene glycol. 93 g (856 mmol) of trimethylsilyl chloride are then added. The reaction medium is stirred at room temperature for 24 hours. After treatment with water, the medium is extracted with ethyl acetate and the organic phases are then combined, dried and concentrated under reduced pressure. The residue obtained is purified by chromatography on a column of silica (eluent: 90 heptane/10 ethyl acetate). A yellow oil is obtained (m=15 g; Y=38%).

後処理

  1. extractionAfter treatment with water, the medium is extracted with ethyl acetate
  2. customdried
  3. concentrationconcentrated under reduced pressure
  4. customThe residue obtained
  5. customis purified by chromatography on a column of silica (eluent: 90 heptane/10 ethyl acetate)
  6. customA yellow oil is obtained (m=15 g; Y=38%)

出典と根拠

ORDレコード
ord-3f22a21e5d8f4203a92994a228ef1806
出典データセット
uspto-grants-2004_03
特許番号
US06706725B1

反応ノート

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