تفاعل #446435

معادلة التفاعل

sodium hydroxide

ammonium peroxodisulfate

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

sulfuric acid

→

1-(2,2-dimethyl-3-oxoindan-1-yl)-5-imidazolecarboxylic acid methyl ester

المردود 60.2%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةis heated to +80° C
2. 2
   درجة الحرارةthe solution is cooled to +7° C.
3. 3
   استخلاصThe solution is extracted twice
4. 4
   تجفيفthe organic phase is dried over sodium sulfate
5. 5
   تركيزconcentrated to dryness by evaporation
6. 6
   workup.ADDITIONis added
7. 7
   ترشيحThe resulting suspension is filtered
8. 8
   تركيزthe filtrate is concentrated by evaporation
9. 9
   أخرىthe residue is crystallised from an ether/hexane mixture

الإجراء التجريبي

A mixture of 30.0 g of 1-(2,2-dimethylindan-1-yl)-5-imidazolecarboxylic acid methyl ester, 150 ml of water and 17 g of sulfuric acid is heated to +80° C. Within a period of 1.5 hours a solution of 114 g of ammonium peroxodisulfate is added dropwise thereto. When the reaction is complete, the solution is cooled to +7° C. and adjusted to pH 3 by the addition of 30% sodium hydroxide solution. The solution is extracted twice using 200 ml of methylene chloride each time, and the organic phase is dried over sodium sulfate and concentrated to dryness by evaporation. The residue is taken up in a small amount of methylene chloride, and ether is added. The resulting suspension is filtered, the filtrate is concentrated by evaporation and the residue is crystallised from an ether/hexane mixture. 19 g of 1-(2,2-dimethyl-3-oxoindan-1-yl)-5-imidazolecarboxylic acid methyl ester having a melting point of 104°-108° C. are obtained.

المصدر