反应详情

温度

0 °C

7.24 parts of 85% powdered potassium hydroxide are added to a solution of 8.2 parts of 2,6-dichloro-4-aminopyrimidine in 200 ml of absolute tetrahydrofuran. The mixture is cooled to 0° C. and then 13.5 parts of 2-chloro-3,5-dinitrobenzotrifluoride in 100 ml of absolute tetrahydrofuran are added in portions, with stirring, over half an hour. During this addition, the colour of the reaction solution turns from yellow to red. The reaction mixture is stirred for 12 hours and then poured into 500 ml of ice-water, acidified with 8 ml of hydrochloric acid, and extracted with two 200 ml portions of ethyl acetate. The combined extracts are washed with 50 ml of water, dried over sodium sulfate, filtered and concentrated. The crude product is crystallised from methanol. Melting point: 198°-200° C.

1. additionDuring this addition
2. stirringThe reaction mixture is stirred for 12 hours
3. extractionextracted with two 200 ml portions of ethyl acetate
4. washThe combined extracts are washed with 50 ml of water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product is crystallised from methanol