反应详情

To a solution of methyl 2-methyl-4-(methyloxy)-3-oxobutanoate (Intermediate 47, 1.01 g, 6.31 mmol) in methanol (7 mL) was added formamidine acetate (0.722 g, 6.94 mmol) and 25% sodium methoxide in MeOH (3.0 mL, 6.31 mmol) and the resulting mixture was heated under reflux for 2 hours, cooled to room temperature and left to stand overnight. The reaction mixture was evaporated under reduced pressure. The residue was diluted with water, adjusted to pH 7 using aqueous 2M HCl solution and extracted with chloroform (×3). The chloroform layers were combined, dried under magnesium sulfate and evaporated under reduced pressure to give the title compound as a white solid (597 mg);

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 2 hours
3. waitleft
4. customThe reaction mixture was evaporated under reduced pressure
5. additionThe residue was diluted with water
6. extractionextracted with chloroform (×3)
7. customdried under magnesium sulfate
8. customevaporated under reduced pressure