反应详情

温度

60 °C

0.7 g of 1-acetyl-3-(1-chloro-1-(4-(imidazol-1-yl-methyl)-phenyl)-methylene)-6-chloro-2-indolinone (educt X.1), 0.4 g of N-(dimethylamino-methylcarbonyl)-N-methyl-p-phenylenediamine (educt XV.125) and 1.2 ml of triethylamine are dissolved in 10 ml of dimethylformamide and stirred for 15 hours at 60° C. After cooling, 10 ml of methanol and 2 ml concentrated ammonia are added and the mixture is stirred for a further three hours at ambient temperature. Water is added and the mixture is extracted with ethyl acetate. The organic phase is washed three times with water, dried over sodium sulphate and concentrated in the rotary evaporator. The residue is purified through a silica gel column with methylene chloride/methanol/ammonia 10:1:0.1 as eluant.

1. temperatureAfter cooling
2. stirringthe mixture is stirred for a further three hours at ambient temperature
3. extractionthe mixture is extracted with ethyl acetate
4. washThe organic phase is washed three times with water
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated in the rotary evaporator
7. customThe residue is purified through a silica gel column with methylene chloride/methanol/ammonia 10:1:0.1 as eluant