Reaktion #991111

ord-a701381362834e3dba288141ded2a620

Reaktionsgleichung

CCCCC(CC)CN
2-ethylhexylamine
CC(C)=CC(=O)Cl
β-methylcrotonyl chloride
CCCCC(CC)CNC(=O)C=C(C)C
N-(2-ethylhexyl)-β-methylcrotonamide
Ausbeute 83.3%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter reaction
  2. 2
    Waschenthe reaction mixture was washed first with diluted hydrochloric acid
  3. 3
    Trocknenwith 10% sodium hydroxide solution and subsequently dried with sodium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off
  5. 5
    workup.DISTILLATIONthe residue was further distilled in vacuum
  6. 6
    Sonstigewas collected

Vorschrift

In 20 ml of n-hexane was dissolved 1.40 g (0.011 mol) of 2-ethylhexylamine. With stirring, 1.20 g (0.01 mol) of β-methylcrotonyl chloride was added to the solution. After reaction, the reaction mixture was washed first with diluted hydrochloric acid and then with 10% sodium hydroxide solution and subsequently dried with sodium sulfate. The solvent was distilled off and the residue was further distilled in vacuum. A fraction having a boiling point of 133°-134° C./l mmHg was collected, obtaining 1.76 g of N-(2-ethylhexyl)-β-methylcrotonamide as an oil (yield: 82.3%). Usual analysis was carried out to identify the compound. The results are shown below.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04229471uspto-grants-1980_10