Reaktion #96021

Reaktionsgleichung

Pyridine

2-aminoethyl methacrylate hydrochloride

diketene

→

acetoacetamidoethyl methacrylate

Ausbeute 60.0%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition
2. 2
   SonstigeThe solvent was then removed at low vacuum
3. 3
   workup.DISSOLUTIONThe residue was dissolved in chloroform (1200 ml)
4. 4
   Waschenwashed with water (twice with 200 ml),
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   Filtrationfiltered
7. 7
   SonstigeExcess solvent was then removed
8. 8
   workup.DISTILLATIONDistillation of the residue

Vorschrift

Pyridine (16 g, 0.2 mole) was added dropwise at 0° C. to a solution of 2-aminoethyl methacrylate hydrochloride (33 g, 0.2 mole) and diketene (16.8 g, 0.2 mole) in N,N-dimethylformamide (600 ml). After the addition, the solution was stirred at 20° C. for 20 hours. The solvent was then removed at low vacuum. The residue was dissolved in chloroform (1200 ml), washed with water (twice with 200 ml), dried over anhydrous magnesium sulfate and filtered. Excess solvent was then removed. Distillation of the residue gave acetoacetamidoethyl methacrylate (b.p.=113°-132° C./5μ) at a yield of 60%.

Quelle