Phthalimide → HCID 66671701, compound

The compound (1.79 g, 3.80 mmol) obtained in Example 91e was dissolved in N,N′-dimethylformamide (60 mL), the mixture was stirred at room temperature, a potassium salt of phthalimide (1.41 g, 7.60 mmol) was added, and the mixture was stirred at 110° C. for 18 hours. After the reaction was completed, saturated aqueous ammonium chloride was added to the reaction mixture under ice cooling, and ethyl acetate was further added to separate the layers. The resulting organic layer was separated, washed with saturated sodium chloride solution, and then dried with anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The resulting residue (3.0 g) was dissolved in ethanol (60 mL), the mixture was stirred at room temperature, hydrazine monohydrate (0.74 mL, 15.2 mmol) was added, and the mixture was stirred at 60° C. for 3.5 hours. After the reaction was completed, the reaction mixture was filtered, and the filtrate was washed with ethyl acetate. The solvent was evaporated under reduced pressure to give the crude title compound (1.71 g) as a pale yellow oily substance.

1. stirringthe mixture was stirred at 110° C. for 18 hours
2. customto separate the layers
3. customThe resulting organic layer was separated
4. washwashed with saturated sodium chloride solution
5. dry with materialdried with anhydrous sodium sulfate
6. customthe solvent was evaporated under reduced pressure
7. dissolutionThe resulting residue (3.0 g) was dissolved in ethanol (60 mL)
8. stirringthe mixture was stirred at room temperature
9. stirringthe mixture was stirred at 60° C. for 3.5 hours
10. filtrationthe reaction mixture was filtered
11. washthe filtrate was washed with ethyl acetate
12. customThe solvent was evaporated under reduced pressure

ORD record

ord-05eef54ff347460ea4ccda1661fe8270

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08476253B2