Reaktion #2302548

Reaktionsgleichung

sodium hydroxide

chloroform

2-(2-amino-2-methyl-propylamino)ethanol

→

1-(2-hydroxyethyl)-3,3,5,5-tetramethylpiperazin-2-one

Lösungsmittel

water

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe temperature of the mixture being maintained at 0°–5° C. during the addition
2. 2
   workup.STIRRINGThe mixture is then stirred at this temperature for further 2 hours and at room temperature for 15 hours
3. 3
   workup.STIRRINGthe mixture is stirred for further 4 hours
4. 4
   FiltrationThen, the mixture is filtered
5. 5
   Waschenthe residue is washed with acetone
6. 6
   WaschenThe filtrate and the acetone of washing
7. 7
   Sonstigeare collected
8. 8
   Sonstigeevaporated under vacuum (70° C./24 mbar)
9. 9
   workup.DISTILLATIONThe residue is distilled
10. 10
    Sonstigegiving a white oil with a boiling point of 115° C. at 2.66 mbar
11. 11
    TemperaturAfter cooling a solid product with a melting point of 91°–93° C.
12. 12
    Sonstigeis obtained

Vorschrift

244.2 g (2.05 mol) of chloroform are added to 180 g (1.36 mol) of 2-(2-amino-2-methyl-propylamino)ethanol in 1204 ml of acetone. The mixture is cooled to 5° C. under stirring and a solution of 327 g (8.18 mol) of sodium hydroxide in 327 ml of water is slowly added, the temperature of the mixture being maintained at 0°–5° C. during the addition. The mixture is then stirred at this temperature for further 2 hours and at room temperature for 15 hours. Subsequently, the pH of the aqueous solution is corrected to 11 and the mixture is stirred for further 4 hours. Then, the mixture is filtered and the residue is washed with acetone. The filtrate and the acetone of washing are collected and evaporated under vacuum (70° C./24 mbar). The residue is distilled giving a white oil with a boiling point of 115° C. at 2.66 mbar. After cooling a solid product with a melting point of 91°–93° C. is obtained.

Quelle