HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 21252869, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 9905551 | HCID 9905551 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 21252869 | HCID 21252869 | 70.4% |
Reaction Steps
9-bromo-5,6-dihydro-2-methoxy-4H-pyrido[3,2,1-jk]carbazole-4-one (1.0 g) obtained in Example 101, step 6 was dissolved in anhydrous dioxane (40 ml), and DDQ (1.45 g) was added at room temperature. The mixture was heated under reflux in an argon atmosphere for 3 hours and allowed to cool. The reaction mixture was added to 1N aqueous solution of sodium hydroxide (150 ml), and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting crude crystals were washed with ethanol and recovered by filtration to obtain the title compound (0.7 g, 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06197768B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-a7af3cdf407b45f68cf1bbdb69753798 |
| Source note | uspto-grants-2001_03 |