Reaktion #70753

ord-7a28caa92ded40cf8e9c99ffc1244f35

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat room temperature
  2. 2
    Temperaturat reflux overnight
  3. 3
    Temperaturcooled
  4. 4
    ExtraktionThe aqueous layer was extracted with ether
  5. 5
    WaschenThe combined organic layers were washed with brine
  6. 6
    Trocknendried over Na2SO4
  7. 7
    Einengenconcentrated in vacuo

Vorschrift

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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536179B2uspto-grants-2013_09