Reaktion #167531

ord-8a0ed242bf0f4cae896fb3334c9ec09f

Reaktionsgleichung

NC(=S)NN/C=C1\N=CC=CC1=O
3-HP
→
C=CC(=O)OCCCC
butyl acrylate
Ausbeute 48.4%

Edukte

NC(=S)NN/C=C1\N=CC=CC1=O
3-HP

Reagenzien

O=S(=O)(O)O
H2SO4

Lösungsmittel

CCCCO
n-butanol

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was refluxed with a Dean-Stark trap
  2. 2
    Sonstigeto remove the water
  3. 3
    Sonstigewas collecting in the Dean-Stark trap
  4. 4
    workup.DISTILLATIONwas distilled off
  5. 5
    Sonstige(0.5 torr, 80° C.)
  6. 6
    workup.DISTILLATIONto distill the remaining liquid

Vorschrift

10.0 g of 30% 3-HP, 100 ml of n-butanol and 5 drops of conc. H2SO4 were mixed in a 250 ml flask. The mixture was refluxed with a Dean-Stark trap attached to remove the water. The refluxing was continued until no more water was collecting in the Dean-Stark trap. A distillation apparatus was attached and most of the n-butanol was distilled off. Next, the temperature was reduced and a vacuum applied (0.5 torr, 80° C.) to distill the remaining liquid. 1.58 g of butyl acrylate was obtained, along with some butanol. The yield of butyl acrylate was 37%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846353B2uspto-grants-2014_09