تفاعل #90652

ord-c81397a6c51d4cf9b7f4f93bfac721c6

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىat room temperature
  2. 2
    درجة الحرارةat reflux overnight
  3. 3
    درجة الحرارةcooled
  4. 4
    استخلاصThe aqueous layer was extracted with ether
  5. 5
    غسيلThe combined organic layers were washed with brine
  6. 6
    تجفيفdried over Na2SO4
  7. 7
    تركيزconcentrated in vacuo

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09446041B2uspto-grants-2016_09