Reaktion #76728

Reaktionsgleichung

hydrochloric acid

lysine hydrochloride

Potassium hydrogencarbonate

sodium chloride

methacryloyl chloride

→

Lysine-methacrylamide

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas further added to the solution
2. 2
   workup.STIRRINGfurther vigorously stirred for about 2 hours
3. 3
   WaschenThe aqueous layer was washed twice with 100 ml of ethyl acetate
4. 4
   Extraktionextracted 3 times with 100 ml of ethyl acetate/isopropanol=1/2
5. 5
   Einengenconcentrated to about 50 ml under reduced pressure
6. 6
   workup.ADDITIONadded with 500 ml of isopropanol
7. 7
   Einengenagain concentrated to about 200 ml
8. 8
   SonstigeThe deposited sodium chloride was removed by filtration
9. 9
   Einengenthe filtrate was concentrated (colorless syrup, 5.53 g)

Vorschrift

Potassium hydrogencarbonate(5.51 g) was dissolved in 100 ml of distilled water, 9.13 g of lysine hydrochloride was dissolved in the solution, and 80 ml of acetone was further added to the solution. The reaction mixture was added dropwise with 5.23 g of methacryloyl chloride over about 10 minutes with vigorous stirring under ice cooling, and further vigorously stirred for about 2 hours. The reaction mixture was adjusted to pH 1-2 with concentrated hydrochloric acid, and saturated with sodium chloride. The aqueous layer was washed twice with 100 ml of ethyl acetate, and extracted 3 times with 100 ml of ethyl acetate/isopropanol=1/2. The ethyl acetate/isopropanol layers were combined, concentrated to about 50 ml under reduced pressure, added with 500 ml of isopropanol, and again concentrated to about 200 ml. The deposited sodium chloride was removed by filtration, and the filtrate was concentrated (colorless syrup, 5.53 g)

Quelle