反应详情

温度

50 °C

A solution of 2-anilino-4-methyl-6-(1-propynyl)-pyrimidine (2.5 g) in dimethyl sulfoxide (2.5 ml) were added to a suspension in 50 ml of tetrahydrofuran of 0.5 g of sodium hydride (60%) of which oily component was removed, and the mixture was stirred at 50° C. for 1 hour. After cooling to room temperature, 1.5 g of chloromethyl ethyl ether was added thereto and the resulting mixture was stirred for 5 hours. The reaction mixture was poured into water and extracted with 150 ml of toluene. The toluene layer was washed wit water, dried over magnesium sulfate and concentrated by evaporation under reduced pressure. The rsidue was purified by silica gel column chromatography to obtain 1.6 g (yield: 62%) of 2-(N-ethoxymethylanilino)-4-methyl-6-(1-propynyl) pyrimidine.

1. customwas removed
2. temperatureAfter cooling to room temperature
3. addition1.5 g of chloromethyl ethyl ether was added
4. stirringthe resulting mixture was stirred for 5 hours
5. additionThe reaction mixture was poured into water
6. extractionextracted with 150 ml of toluene
7. washThe toluene layer was washed wit water
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated by evaporation under reduced pressure
10. customThe rsidue was purified by silica gel column chromatography