反応 #8989

反応方程式

ammonium sulfate

2-acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester

hexamethyldisilazane

→

desired compound

1-Cyclopropyl-2,5-dimethyl-1H-imidazole-4-carboxylic acid ethyl ester

反応条件

後処理

1. 1
   その他The reaction mixture was evaporated
2. 2
   抽出extracted with ethyl acetate and water
3. 3
   乾燥The organic phase was dried over sodium sulfate
4. 4
   その他evaporated
5. 5
   その他The crude product was purified by column chromatography on silica gel (ethyl acetate/methanol 4:1)

実験手順

Fine powdered ammonium sulfate (0.13 g, 1 mmol) was added to a suspension of Z)-2-acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester (7.0 g, 20 mmol) and hexamethyldisilazane (50 ml, 235 mmol) and refluxed over night at 145° C. The reaction mixture was evaporated and extracted with ethyl acetate and water. The organic phase was dried over sodium sulfate and evaporated. The crude product was purified by column chromatography on silica gel (ethyl acetate/methanol 4:1) and the desired compound was obtained as a light brown solid (1.3 g, 31%), MS: m/e=209.1 (M+H+).

出典