반응 #5869

반응 방정식

1-(2,2-dimethyl-tetralin-1-yl)-5-imidazolecarboxylic acid methyl ester

sodium hydroxide

→

1-(2,2-dimethyl-4-oxo-tetralin-1-yl)-5-imidazolecarboxylic acid methyl ester

수율 28.2%

용매

water

반응 조건

후처리

1. 1
   온도The suspension is heated to +87° C.
2. 2
   workup.ADDITIONwithin a period of 1.5 hours a total of 335 g of ammoniaperoxodisulfate is added portionwise in such a manner
3. 3
   기타does not exceed +90° C
4. 4
   온도After cooling the reaction mixture to +15° C.
5. 5
   추출The mixture is extracted with 500 ml of methylene chloride
6. 6
   기타The organic phase is separated
7. 7
   건조dried with sodium sulfate
8. 8
   workup.ADDITIONtreated with activated carbon
9. 9
   농축concentrated
10. 10
    기타Crystallisation of the residue from diethyl ether

실험 절차

142 g of 1-(2,2-dimethyl-tetralin-1-yl)-5-imidazolecarboxylic acid methyl ester are dispersed in 1 liter of deionisized water. The suspension is heated to +87° C., and within a period of 1.5 hours a total of 335 g of ammoniaperoxodisulfate is added portionwise in such a manner, that the temperature does not exceed +90° C. After cooling the reaction mixture to +15° C., the pH-value is adjusted to pH 4 by addition of 335 g of a sodium hydroxide solution 30%. The mixture is extracted with 500 ml of methylene chloride. The organic phase is separated, dried with sodium sulfate, treated with activated carbon and concentrated. Crystallisation of the residue from diethyl ether yields 42 g of 1-(2,2-dimethyl-4-oxo-tetralin-1-yl)-5-imidazolecarboxylic acid methyl ester, having a melting point of 93°-95° C.

출처