반응 #75307

반응 방정식

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

용매

methylene chloride

반응 조건

후처리

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

실험 절차

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.

출처