反応 #446437

反応方程式

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

収率 28.2%

溶媒

water

反応条件

後処理

1. 1
   温度The suspension is heated to +87° C.
2. 2
   温度After the reaction mixture has been cooled to +15° C.
3. 3
   抽出the whole is extracted with 500 ml of methylene chloride
4. 4
   その他The organic phase is separated off
5. 5
   乾燥dried over sodium sulfate
6. 6
   workup.ADDITIONtreated with activated carbon
7. 7
   濃縮concentrated by evaporation
8. 8
   その他Crystallisation of the residue from ether

実験手順

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.

出典