反应详情

2.48 g (13.0 mmol) 6-chloro-2-methyl-pyrimidine-4-carboxylic acid chloride, 1.94 g (13.0 mmol) 4-methyl-3H-benzoxazol-2-one and 6.93 g (52.0 mmol) aluminium trichloride were heated to 125° C. for 1.5 h with stirring. The mixture was combined with ice water and the precipitate formed was suction filtered and washed with water. Then the precipitate was dissolved in MeOH/DCM and filtered through silica gel suction. The filtrate was evaporated down and the residue was purified by flash chromatography. The fractions containing the product were combined, evaporated down and triturated with diethyl ether. The precipitate was suction filtered, washed with diethyl ether and dried i. vac.

1. customthe precipitate formed
2. filtrationfiltered
3. washwashed with water
4. dissolutionThen the precipitate was dissolved in MeOH/DCM
5. filtrationfiltered through silica gel suction
6. customThe filtrate was evaporated down
7. customthe residue was purified by flash chromatography
8. additionThe fractions containing the product
9. customevaporated down
10. customtriturated with diethyl ether
11. filtrationfiltered
12. washwashed with diethyl ether
13. customdried i