反应详情

A solution of 0.22 g of the acid from Step C was refluxed in thionyl chloride for 1 hour followed by removal of the solvent under vacuum to give an oil. The oil was dissolved in 1 mL of methylene chloride and added to a solution of 2-aminomethyl-3-chloro-5-trifluoromethylpyridine hydrochloride (0.25 g) and triethylamine (0.20 g) in 9 mL of methylene chloride at room temperature. The reaction mixture was stirred at room temperature overnight. The reaction mixture was then filtered through silica gel, eluting with 100% methylene chloride. Removal of the solvent under vacuum provided the title compound as a solid, m.p. 122-124° C.

1. customfollowed by removal of the solvent under vacuum
2. customto give an oil
3. filtrationThe reaction mixture was then filtered through silica gel
4. washeluting with 100% methylene chloride
5. customRemoval of the solvent under vacuum