反应详情

1-Acetyl-1,2-dihydroindol-3-one of Example 1d (131.3 g, 0.75 mol) and 5,5-dimethyl-cyclohexane-1,3-dione (105 g, 0.75 mol) were added to a mixture of acetic acid (700 mL) and triethylamine (105 mL, 0.75 mol) at room temperature under stirring. The reaction mixture was refluxed for 6 h. About ⅓ volume of solvents was removed in vacuum, and the mixture was cooled and diluted with water (50 mL). The precipitate was filtered off, washed with ethanol-water, 1:1 and dried to afford 169.4 g (76%) of colorless crystals; m.p. 225-227° C.

1. temperatureThe reaction mixture was refluxed for 6 h
2. customAbout ⅓ volume of solvents was removed in vacuum
3. temperaturethe mixture was cooled
4. additiondiluted with water (50 mL)
5. filtrationThe precipitate was filtered off
6. washwashed with ethanol-water, 1:1
7. customdried