反应详情

A solution of 5-(bis(2,2,2-trifluoroethyl)amino)-6-(cyclopropylmethoxy)-pyridine-2-carboxylic acid methyl ester (60 mg, 0.16 mmol) and sodium hydroxide (9 mg, 0.23 mmol) in ethanol (20 mL) was reacted for 2 h at 90° C. The reaction mixture was concentrated under reduced pressure, dissolved in water and extracted with ethyl acetate (10 mL). The pH of the aqueous layer was adjusted to 2 by addition of 1 N hydrochloric acid; the aqueous layer was extracted with ethyl acetate (3×10 mL), washed with brine (2×10 mL), dried over Na2SO4 and evaporated to dryness (0.03 g, crude). The crude product was used for next step without further purification; MS: m/e=373.1 [M+H]+.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutiondissolved in water
3. extractionextracted with ethyl acetate (10 mL)
4. additionThe pH of the aqueous layer was adjusted to 2 by addition of 1 N hydrochloric acid
5. extractionthe aqueous layer was extracted with ethyl acetate (3×10 mL)
6. washwashed with brine (2×10 mL)
7. dry with materialdried over Na2SO4
8. customevaporated to dryness (0.03 g, crude)
9. customThe crude product was used for next step without further purification