反应详情

After dissolving 3.25 g of chloromethyl-dimethyl(4-fluorobenzyl)silane in 10 ml of xylene, 2.55 g of imidazole are added to the solution which is then refluxed for 12 hours. After adding 50 ml of water to the mixture and separating, the organic phase is washed with a total of 100 ml of water in 5 portions. The organic phase is dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated to solvent-free. The pale yellow oily residue is dissolved in 20 ml of ethyl acetate and gaseous hydrogen chloride is introduced to the solution until reaching a pH value of 4 to 5. The precipitated crystalline product name is filtered in two portions at 10° C. and washed with a total of 6 ml of ethyl acetate to give the named compound in a yield of 3.41 g (80%), m.p.: 152°-154° C.

1. additionare added to the solution which
2. temperatureis then refluxed for 12 hours
3. customseparating
4. washthe organic phase is washed with a total of 100 ml of water in 5 portions
5. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customthe filtrate is evaporated to solvent-free
8. dissolutionThe pale yellow oily residue is dissolved in 20 ml of ethyl acetate
9. additiongaseous hydrogen chloride is introduced to the solution
10. filtrationThe precipitated crystalline product name is filtered in two portions at 10° C.
11. washwashed with a total of 6 ml of ethyl acetate
12. customto give the named compound in a yield of 3.41 g (80%), m.p.: 152°-154° C.