反应详情

Bromine (1.22 g, 7.6 mmol) in acetic acid (5.6 ml) is added to a solution of 4-Fluoro-2-(2-methylthio-4-pyrimidyl)acetophenone (2 g; 7.6 mmol) in acetic acid (40 ml. The initially thick precipitate is almost dissolved after 20 min, filtered and the filtrate evaporated to dryness. The residue is taken up in a saturated solution of NaHCO3 and extracted three times with tert.butyl methyl ether. The combined organic phases are dried over Na2SO4 and evaporated to dryness to yield 2.6 g (100%) of a brown oil, which is used in the next step without purification.

1. dissolutionThe initially thick precipitate is almost dissolved after 20 min
2. filtrationfiltered
3. customthe filtrate evaporated to dryness
4. extractionextracted three times with tert.butyl methyl ether
5. dry with materialThe combined organic phases are dried over Na2SO4
6. customevaporated to dryness