تفاعل #446437

معادلة التفاعل

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

ammonium peroxodisulfate

sodium hydroxide

→

1-(2,2-dimethyl-4-oxotetralin-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
   درجة الحرارةAfter the reaction mixture has been cooled to +15° C.
3. 3
   استخلاصthe whole is extracted with 500 ml of methylene chloride
4. 4
   أخرىThe organic phase is separated off
5. 5
   تجفيفdried over sodium sulfate
6. 6
   workup.ADDITIONtreated with activated carbon
7. 7
   تركيزconcentrated by evaporation
8. 8
   أخرىCrystallisation of the residue from ether

الإجراء التجريبي

142 g of 1-(2,2-dimethyltetralin-1-yl)-5-imidazolecarboxylic acid methyl ester are suspended in 1 liter of distilled water. The suspension is heated to +87° C. and, while stirring, a total of 335 g of ammonium peroxodisulfate is added in portions thereto within a period of 1.5 hours in such a manner that the temperature does not exceed +90° C. After the reaction mixture has been cooled to +15° C., the pH value is adjusted to pH 4 by the addition of approximately 335 g of 30% sodium hydroxide solution and the whole is extracted with 500 ml of methylene chloride. The organic phase is separated off, dried over sodium sulfate, treated with activated carbon and concentrated by evaporation. Crystallisation of the residue from ether yields 42 g of 1-(2,2-dimethyl-4-oxotetralin-1-yl)-5-imidazolecarboxylic acid methyl ester having a melting point of 93°-95° C.

المصدر