Reaktion #75105

Reaktionsgleichung

dimethyl 6-chloro-2,4-pyrimidine-dicarbamate-3-oxide

4-hydroxy-piperidine

→

dimethyl racemic-6-(4-hydroxy-1-piperidinyl)-2,4-pyrimidine-dicarbamate-3-oxide

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA suspension of 2.5 g
2. 2
   FiltrationThe separated precipitate is filtered off
3. 3
   Sonstigerecrystallized from a mixture of methylene chloride and methanol, there

Vorschrift

A suspension of 2.5 g. of dimethyl 6-chloro-2,4-pyrimidine-dicarbamate-3-oxide in 100 ml. of methylene chloride is treated with 10 g. of 4-hydroxy-piperidine and stirred at room temperature under an argon atmosphere for 70 hours. The separated precipitate is filtered off and recrystallized from a mixture of methylene chloride and methanol, there being obtained pure dimethyl racemic-6-(4-hydroxy-1-piperidinyl)-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 265°-266° C.

Quelle