反应详情

温度

22 °C

To a solution of 2,6-diacetylpyridine (35 g, 0.21 mol) in THF (1.21) was added 2-chloro-4,6-dimethylaniline (76.7 g, 2.3 eq) and Sicapent (45 g). The reaction mixture was refluxed overnight. Then additional 2-chloro-4,6-dimethylaniline (25 g, 0.7 eq) and Sicapent (25 g) were added and once again refluxed overnight. The suspension was cooled to 22° C., filtered and washed with two times THF (75 ml). The mother liquor was concentrated (90%) and methanol was added to precipitate the product, which was washed two times with methanol (50 ml) and dried under high vacuum. 68.8 g of a yellow powder was isolated (y=73.1%)

1. temperatureThe reaction mixture was refluxed overnight
2. filtrationfiltered
3. washwashed with two times THF (75 ml)
4. concentrationThe mother liquor was concentrated (90%) and methanol
5. additionwas added
6. customto precipitate the product, which
7. washwas washed two times with methanol (50 ml)
8. customdried under high vacuum