反应详情

温度

-40 °C

Dissolve 2-amino-4-chloronicotinaldehyde (78 mg, 0.5 mmol) and 2-acetyl-5-amino-3-trifluoromethylpyridine (102 mg, 0.5 mmol) in anhydrous THF (5.0 mL) and cool it to −40° C. under N2 atmosphere. Add in portion t-BuOK (112 mg, 1.0 mmol) to the reaction mixture and stir the mixture at −110° C. for 2 hours. Concentrate the reaction mixture under vacuum, dilute the residue with water (20 mL), extract with CH2Cl2 (3×30 mL) and dry (MgSO4). Filter, concentrate under vacuum and purify the crude by column chromatography to afford the title compound product as a yellow solid.

1. concentrationConcentrate the reaction mixture under vacuum
2. additiondilute the residue with water (20 mL)
3. extractionextract with CH2Cl2 (3×30 mL)
4. dry with materialdry (MgSO4)
5. filtrationFilter
6. concentrationconcentrate under vacuum
7. custompurify the crude by column chromatography