反应详情

温度

25 °C

A suspension of 9-oxo-5,6,7,8,9,10-hexahydro-acridine-3-carboxylic acid (1 g, 0.42 mmols) in toluene (10 mL) was heated with phosphorous oxybromide (3.54 g, 1.2 mmols) to 100° C. for 4 h. Reaction completion was monitored by TLC. Alter completion, the reaction mixture was cooled to 25° C., quenched with methanol (10 mL), concentrated the reaction mixture under vacuum and purified the crude product with silica gel column (60:120). Product eluted with 2% methanol in chloroform. Fractions were collected and concentrated to get the pure product as off white solid. This compound was taken as such to next step.

1. customReaction completion
2. customquenched with methanol (10 mL)
3. concentrationconcentrated the reaction mixture under vacuum
4. custompurified the crude product with silica gel column (60:120)
5. washProduct eluted with 2% methanol in chloroform
6. customFractions were collected
7. concentrationconcentrated
8. customto get the pure product as off white solid