反应详情

温度

150 °C

A mixture of 3-anilino-2-naphthoic acid (10.0 g, 37.98 mmol) and phosphorous oxychloride (35.4 ml, 379.8 mmol) was refluxed at 150° C. under nitrogen with stirring for 2 hours. The resulting purple mixture was cooled and evaporated under reduced pressure to dryness. The content was added with stirring to a mixture of chloroform/ice/conc. ammonium hydroxide (200 ml/200 g/200 ml). The chloroform layer was separated and dried over calcium chloride. Removal of the solvent under reduced pressure gave -12-chlorobenz-[b]acridine (9.4 g, 95%). Rf 0.8 (silica gel, hexane/ethyl acetate 2:1). MS (EI): m/z 263 (M).

1. temperatureThe resulting purple mixture was cooled
2. customevaporated under reduced pressure to dryness
3. additionThe content was added
4. stirringwith stirring to a mixture of chloroform/ice/conc
5. customThe chloroform layer was separated
6. dry with materialdried over calcium chloride
7. customRemoval of the solvent under reduced pressure