Reaktion #48030

Reaktionsgleichung

N,N-dimethyl-N′-phenyl-chloroformamidine

1-aminooxy-2-hydroxy-3-(1-piperidinyl)-propane

Na2CO3

→

N,N-dimethyl-N′-[2-hydroxy-3-(1-piperidinyl)-propoxy]-N″-phenyl-guanidine hydrochloride

Lösungsmittel

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationAfter 5 hours the solid state was filtered
2. 2
   Sonstigethe filtrate was evaporated
3. 3
   workup.DISSOLUTIONThis residue (1800 mg oil) was dissolved in 10 ml of ethyl acetate
4. 4
   Sonstigethe product was precipitated by addition of 10.46 ml of 0.54 N HCl/ethyl acetate
5. 5
   FiltrationThe yellow precipitate was filtered off
6. 6
   Waschenwashed
7. 7
   Sonstigefinally recrystallized from acetone

Vorschrift

1150 mg (6.58 mmole) of 1-aminooxy-2-hydroxy-3-(1-piperidinyl)-propane (Ger. Off. 2 651 083) was dissolved in chloroform and 750 mg of Na2CO3 was added, then a solution of 1206 mg (6.58 mmole) of N,N-dimethyl-N′-phenyl-chloroformamidine (BR 888646/1959, Bayer, auth.: Kühle and Eue L.; CA 57, 136961/1962/) in 10 ml of chloroform was added dropwise. After 5 hours the solid state was filtered and the filtrate was evaporated. This residue (1800 mg oil) was dissolved in 10 ml of ethyl acetate, and the product was precipitated by addition of 10.46 ml of 0.54 N HCl/ethyl acetate. The yellow precipitate was filtered off, washed, and finally recrystallized from acetone, after ethyl acetate.

Quelle