Ethanol → Ethyl cyclobutanecarboxylate

HRID 42475

反応式

HRID 42475 の反応式
[CH:1]1([C:5]([OH:7])=[O:6])[CH2:4][CH2:3][CH2:2]1.OS(O)(=O)=O.O.[CH3:14][CH2:15]O>>[CH:1]1([C:5]([O:7][CH2:14][CH3:15])=[O:6])[CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 4

HCID 702EthanolHCID 962WaterHCID 1118Sulfuric AcidHCID 19494Cyclobutanecarboxylic acid

生成物 1

HCID 84700Ethyl cyclobutanecarboxylate収率 69%

実験手順

To a solution of cyclobutanecarboxylic acid (50 g, 500 mmol) in EtOH (1.2 L) was slowly added H2SO4 (20 mL) at room temperature. The solution was stirred at reflux overnight, and then cooled and poured into H2O. The aqueous layer was extracted with ether. The combined organic layers were washed with brine, dried over Na2SO4, and concentrated in vacuo to give ethyl cyclobutanecarboxylate as a colorless oil (44 g, 69%). 1H NMR (400 MHz, CDCl3-d3) δ 4.04 (q, 2H), 3.04 (m, 1H), 2.12 (m, 4H), 1.88 (m, 2H), 1.18 (t, 3H).

後処理

  1. customat room temperature
  2. temperatureat reflux overnight
  3. temperaturecooled
  4. extractionThe aqueous layer was extracted with ether
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7a28caa92ded40cf8e9c99ffc1244f35
出典データセット
uspto-grants-2013_09
特許番号
US08536179B2

関連ノート

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