Ethanol → HCID 178518912, compound

Participants

Reaction Steps

To the product of step 3 in 3.0 mL of EtOH at 0° C. was added anhydrous hydrazine (0.16 mL, 5.1 mol). The ice bath was removed, and the homogeneous solution was stirred at RT for 15 min, then the EtOH was removed by rotovap. To the remaining mixture at RT was added 2.0 mL of glacial acetic acid, and the mixture stirred at RT for 5 min, then in an oil bath at 95° C. for 10 min. It was cooled to RT, and treated with 3 mL of water. The precipitated yellow solid was filtered, rinsed with 2×1 mL of water followed by 2×1 mL of ether. The solid was dried in a vacuum oven at 45° C. for 18 h, to afford 2-(2,4-difluorophenylamino)pyrido[3,2-d]pyridazin-5-ol as a yellow crystalline solid. MS (ESI, pos.ion) m/z: M+1=275.1

Provenance & Evidence