Реакция #89620

ord-eba05cae420d4eb5ae930194eb321a31

Реагенты

Нет

Условия реакции

Температура
150°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe autoclave was sealed
  2. 2
    ТемператураThe temperature of the autoclave increased to 195° C. due to the
  3. 3
    Температураheat of the reaction
  4. 4
    Другоеthe completion of the reaction
  5. 5
    ТемператураThe autoclave was then cooled to room temperature
  6. 6
    workup.DISTILLATIONSimple distillation of the resulting mixture

Методика

Isoprene (350 g, 5.1 mol) and dimethyl maleate (741 g, 5.1 mol) were loaded into a stainless steel autoclave. The autoclave was sealed and heated to 150° C. The temperature of the autoclave increased to 195° C. due to the heat of the reaction. The temperature was held at 160° C. for 1 hour. Gas chromatography (GC) analysis indicated the completion of the reaction. The autoclave was then cooled to room temperature. Simple distillation of the resulting mixture provided 4-methyl-cyclohex-4-ene-1,2-dicarboxylic acid dimethyl ester (725 g, 3.4 mol, 66% yield) as a light yellow liquid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09441185B2uspto-grants-2016_09