HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22449736, compound → HCID 22449621, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22449736 | HCID 22449736 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22449621 | HCID 22449621 | 69% |
Reaction Steps
2,4-Dioxo-1-[4-(4-diphenylmethoxypiperidino)butyl]-7-nitro-1,2,3,4-tetrahydroquinazoline (3.00 g) obtained in Example 11 was dissolved in a mixture of concentrated hydrochloric acid (10.0 ml), water (50.0 ml), ethanol (50.0 ml) and tetrahydrofuran (50.0 ml) and an excess of zinc powder was added in portions. After completion of the reaction, the reaction mixture was filtered, and the filtrate was made basic with 25% aqueous ammonia solution and 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 (1.95 g, 69%). Recrystallization from ethyl acetate yielded a yellow crystal having a melting point of 162 to 164° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06407116B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-6e05179d912840f69a40df3cad2614b3 |
| Source note | uspto-grants-2002_06 |