Ethylene Glycol → Ethyl 2-methyl-1,3-dioxolane-2-propionate

HRID 1627780

反応式

HRID 1627780 の反応式
[C:1]([O:8][CH2:9][CH3:10])(=[O:7])[CH2:2][CH2:3][C:4]([CH3:6])=[O:5].[CH2:11](O)[CH2:12][OH:13].C1(C)C=CC(S(O)(=O)=O)=CC=1.[NH+]1C=CC=CC=1.O>C1(C)C=CC=CC=1>[CH3:6][C:4]1([CH2:3][CH2:2][C:1]([O:8][CH2:9][CH3:10])=[O:7])[O:13][CH2:12][CH2:11][O:5]1

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 962WaterHCID 10883Ethyl levulinateHCID 22033616Pyridinium.p-toluenesulfonate

生成物 1

HCID 70332Ethyl 2-methyl-1,3-dioxolane-2-propionate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

In a flask equipped by a Dean-Stark trap, a mixture of ethyl levulinate (28.83 g; 200 mmol), ethylene glycol (37.24 g; 600 mmol) and a catalytic amount of pyridinium para-toluenesulfonic acid in toluene (200 mL) was heated at reflux until the theoretical amount of water was distilled off. After cooling, the mixture was washed with a saturated solution of sodium hydrogenocarbonate. The basic layer was extracted with diethylether and the organics were combined, then washed with brine and water. The organic layer was dried over sodium sulphatesulphate and concentrated under reduced pressure to afford the ethyl 3-(2-methyl-1,3-dioxolan-2-yl)propanoate as a colorless oil.

後処理

  1. customIn a flask equipped by a Dean-Stark trap
  2. distillationwas distilled off
  3. temperatureAfter cooling
  4. washthe mixture was washed with a saturated solution of sodium hydrogenocarbonate
  5. extractionThe basic layer was extracted with diethylether
  6. washwashed with brine and water
  7. dry with materialThe organic layer was dried over sodium sulphatesulphate
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ef41ac51bcf841e29afb641fc0b8899b
出典データセット
uspto-grants-2014_07
特許番号
US08785638B2

関連ノート

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