反应详情

温度

2.5 °C

To a 50 L three-neck round bottom flask, equipped with a mechanical stirrer, addition funnel and thermometer, were added 2-methyl-1H-indol-5-ol (compound 1, 3 Kg), anhydrous acetonitrile (9 L) and potassium carbonate (4.2 Kg). The reaction mixture was cooled to 0-5° C. with stirring under N2. A solution of 2,4-dichloropyrimidine (Compound 2, 3.05 Kg, in 9 L of acetonitrile) was added to the reaction mixture dropwise while keeping the inner temperature of the reaction in the range from 0 to 5° C. After addition was complete, the reaction mixture was allowed to warm to a temperature ranging from 5 to 10° C. over a period of 4-8 hours. When reaction was completed, the reaction mixture was poured into 54 L of distilled water in a 100 L reactor with stirring, and stirred for another hour at room temperature. The precipitates were collected by filtration and the filter cake was washed with pure water to afford Compound 3 (5.7 Kg).

1. customTo a 50 L three-neck round bottom flask, equipped with a mechanical stirrer, addition funnel
2. customthe inner temperature of the reaction in the range from 0 to 5° C
3. additionAfter addition
4. temperatureto warm to a temperature
5. customWhen reaction
6. stirringwith stirring
7. stirringstirred for another hour at room temperature
8. filtrationThe precipitates were collected by filtration
9. washthe filter cake was washed with pure water