Reaktion #76729

Reaktionsgleichung

hydrochloric acid

arginine hydrochloride

Potassium hydrogencarbonate

sodium chloride

methacryloyl chloride

→

Arginine-methacrylamide

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas further added to the solution
2. 2
   workup.STIRRINGfurther vigorously stirred for 1 hour
3. 3
   WaschenThe aqueous layer was washed 3 times with 300 ml of ethyl acetate
4. 4
   Extraktionextracted 3 times with 200 ml of ethyl acetate/isopropanol =1/1
5. 5
   Einengenconcentrated to about 100 ml under reduced pressure
6. 6
   workup.ADDITIONadded with 400 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, 21.80 g)

Vorschrift

Potassium hydrogencarbonate(27.64 g) was dissolved in 200 ml of distilled water, 21.07 g of arginine hydrochloride was dissolved in the solution, and 80 ml of acetone was further added to the solution. The reaction mixture was added dropwise with 10.46 g of methacryloyl chloride over about 10 minutes with vigorous stirring under ice cooling, and further vigorously stirred for 1 hour. The reaction mixture was adjusted to pH 1 with concentrated hydrochloric acid, and saturated with sodium chloride. The aqueous layer was washed 3 times with 300 ml of ethyl acetate, and extracted 3 times with 200 ml of ethyl acetate/isopropanol =1/1. The ethyl acetate/isopropanol layers were combined, concentrated to about 100 ml under reduced pressure, added with 400 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, 21.80 g)

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