تفاعل #5869

معادلة التفاعل

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

المردود 28.2%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe 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
   أخرىdoes not exceed +90° C
4. 4
   درجة الحرارةAfter cooling the reaction mixture to +15° C.
5. 5
   استخلاصThe mixture is extracted with 500 ml of methylene chloride
6. 6
   أخرىThe organic phase is separated
7. 7
   تجفيفdried with sodium sulfate
8. 8
   workup.ADDITIONtreated with activated carbon
9. 9
   تركيزconcentrated
10. 10
    أخرىCrystallisation of the residue from diethyl ether

الإجراء التجريبي

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.

المصدر