反应详情

温度

100 °C

A mixture of 5-amino-1,3-dimethylpyridin-2(1H)-one (Step 20.2) (1.77 g, 12.78 mmol), 4-chlorobenzaldehyde (1.63 g, 11.62 mmol) and ethyl 4-cyclopropyl-2,4-dioxobutanoate (2 g, 11.62 mmol) in acetic acid (10 mL) was stirred for 2 h at 100° C. The reaction mixture was concentrated, diluted with CH2Cl2/1 N NaOH, and extracted with CH2Cl2. The combined organic extracts were discarded. The aqueous layer was acidified to pH 3 with 6 N HCl and extracted twice with CH2Cl2. The combined organic extracts were dried (Na2SO4) and concentrated to afford 3.06 g of the title compound as a beige foam. tR. 0.83 min (LC-MS 2); ESI-MS: 387.0 [M+H]+ (LC-MS 2).

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with CH2Cl2/1 N NaOH
3. extractionextracted with CH2Cl2
4. extractionextracted twice with CH2Cl2
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. concentrationconcentrated