反应详情

温度

0 °C

Anhydrous dichloromethane (750 ml) and 2-chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine (18.84 g) were combined and cooled to 0° C. Triethylamine (12.9 ml) was added dropwise to the resulting mixture, and then ethoxyacetyl chloride (11.34 g) dissolved in anhydrous dichloromethane (50 ml) was added slowly to the resulting mixture, which turned dark. After two hours the dark mixture was allowed to warm to room temperature. TLC analysis of the reaction mixture indicated completion, and the solvent was removed under reduced pressure. The resulting yellow solid was dissolved in chloroform, and the resulting solution was washed with water. The organic layer was dried with magnesium sulfate and concentrated to a dark brown oil (27.75 g) under reduced pressure. NMR analysis of the oil indicated desired product of suitable purity for use in the next step.

1. additionwas added slowly to the resulting mixture, which
2. temperatureto warm to room temperature
3. customthe solvent was removed under reduced pressure
4. dissolutionThe resulting yellow solid was dissolved in chloroform
5. washthe resulting solution was washed with water
6. dry with materialThe organic layer was dried with magnesium sulfate
7. concentrationconcentrated to a dark brown oil (27.75 g) under reduced pressure