Ethanol → HCID 15894616, compound

Participants

Reaction Steps

To a boiled ethanol solution (300 mL) of 7-benzoyl-1-ethoxycarbonylphenazine 5-oxide (4.00 g, 10.7 mmol. obtained in Reference Example 1) was dropwise added for a period of one hour an aqueous solution (150 mL) of 85% sodium hydrosulfate (8.86 g, 43.2 mol.) in gaseous nitrogen atmosphere. After the dropwise addition was complete, the reaction mixture was further heated under reflux for 10 minutes. The refluxed mixture was then cooled to room temperature. To the cooled mixture was added water (150 mL). Thus deposited crystalline product was collected by filtration and washed with water. The washed product was placed under reduced pressure at 40° C. for 16 hours in the presence of diphosphorus pentoxide to dryness. Thus, 3.10 g (81%) of the desired compound was obtained as a brown-violet crystalline product. mp: 175-177° C.

Provenance & Evidence