反应详情

A solution of 2-[3-(2,2a,4,5-Tetrahydro-1H-3-aza-acenaphthylen-3-yl)-propyl]-isoindole1,3-dione (2 g, 5.78 mmol) and hydrazine hydrate (2.9 g, 57.8 mol) in ethanol (60 mL) was refluxed for 1 h. The reaction mixture was cooled down and treated with an additional amount of ethanol (30 mL) and concentrated HCl (7 mL). Then the reaction mixture was refluxed for 4 h and left overnight in a refrigerator. The precipitate was filtered off, and the solvent was evaporated. The residue was redissolved in water (15 ml) and made alkaline with 25% ammonia. Then, was extracted with CH2Cl2 (3×120 mL), the organic layer was dried over Na2SO4, and evaporated to dryness. The crude was dissolved in ethylacetate. A 2.8 M solution of hydrogen chloride in ethanol was then added. The precipitate formed was collected by filtration to give the desired product (0.80 g, 64% yield) as a beige solid.

1. temperatureThe reaction mixture was cooled down
2. temperatureThen the reaction mixture was refluxed for 4 h
3. filtrationThe precipitate was filtered off
4. customthe solvent was evaporated
5. dissolutionThe residue was redissolved in water (15 ml)
6. extractionThen, was extracted with CH2Cl2 (3×120 mL)
7. dry with materialthe organic layer was dried over Na2SO4
8. customevaporated to dryness
9. dissolutionThe crude was dissolved in ethylacetate
10. additionA 2.8 M solution of hydrogen chloride in ethanol was then added
11. customThe precipitate formed
12. filtrationwas collected by filtration