Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 70154155 | HCID 70154155 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22449885 | HCID 22449885 | 19% |
Reaction Steps
Ethyl N-[2,4-dioxo-1-[4-(4-diphenylmethoxypiperidino)butyl]-1,2,3,4-tetrahydro-7-quinazolinyl]malonamide (690 mg) obtained in Example 43 was dissolved in tetrahydrofuran (10.0 ml) and ethanol (10.0 ml) and then a 1N aqueous solution of sodium hydroxide (5.0 ml) was added. The reaction mixture was stirred at room temperature for 16 hours and the solvent was distilled off under reduced pressure, and the residue was made acidic with 1N hydrochloric acid, and then extracted with ethyl acetate. After the extract was washed with water and dried (Na2SO4), the solvent was distilled off under reduced pressure to give the title compound (126 mg, 19%). Recrystallization from ethyl acetate-methanol-tetrahydrofuran yielded a colorless crystal having a melting point of 230 to 232° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06407116B1 |
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| Source dataset | uspto-grants-2002_06 |
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| ORD ID | ord-56eedfa83bc6411d8049f1ea14dc0535 |
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| Source note | uspto-grants-2002_06 |
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