Реакция #2203925

ord-619dec1ca69149a4b70f3f0d560f1bfb

Условия реакции

Температура
230°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеequipped with a distillation column, condenser
  2. 2
    workup.ADDITIONthe following constituents were added
  3. 3
    ДругоеAt a batch temperature of 180° C.
  4. 4
    Другоеwas removed
  5. 5
    ТемператураThe batch temperature was then raised to 200° C.
  6. 6
    workup.ADDITIONthe pressure dropped to 267 Pa
  7. 7
    workup.WAITDuring this period
  8. 8
    Другоеa cut of 140.9 g of the amide acetal was recovered

Методика

To a 1 liter stirred reactor, equipped with a distillation column, condenser, and graduated receiver, the following constituents were added: 261.2 g of diisopropanol amine (DIPA) and 432.0 g (98%) of methyl laurate. The contents were heated slowly to 230° C. under a nitrogen blanket. After 5.5 hours, 57 ml of methanol (0.72 equivalent) had come overhead. The pressure was then slowly lowered to strip out unreacted DIPA. At a batch temperature of 180° C. and a pressure of 293 Pa, a cut consisting of 79.7 g of DIPA and 87.8 g of methyl laurate was removed. The batch temperature was then raised to 200° C. and the pressure dropped to 267 Pa. During this period, a cut of 140.9 g of the amide acetal was recovered. This represents a 35.7% conversion of the methyl laurate to amide acetal.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07439354B2uspto-grants-2008_10