反应详情

At 26° C., combine triethylsilane (110 g, 946 mmol) and (4-chloro-2-fluorophenyl)(6-chloro-2-methyl-8-(morpholinomethyl)imidazo[1,2-b]pyridazin-3-yl)methanone (50.1 g, 117.06 mmol) to form a solution. Add trifluoro acetic acid (150 mL, 1.98 mol) to the reaction mixture then heat at 78° C. for 24 h. Cool the reaction to ambient temperature and separate the mixture to remove the top layer. Dissolve the bottom layer with ethyl acetate (1 L) and adjust the pH to 11 with sodium hydroxide (4 N, 500 mL). Separate the organic layer and add HCl (4 M in ethyl ether) to the organic layer to form the HCl salt. Filter and dry the HCl salt. (100 g (96%); mp=237-238° C.; M+=409).

1. customAt 26° C.
2. customto form a solution
3. temperatureCool
4. customthe reaction to ambient temperature
5. customseparate the mixture
6. customto remove the top layer
7. dissolutionDissolve the bottom layer with ethyl acetate (1 L)
8. customSeparate the organic layer
9. additionadd HCl (4 M in ethyl ether) to the organic layer