反应详情

温度

80 °C

To a solution of o-phenylenediamine (2 g) in propyl orthocarbonate (5 ml) was added acetic acid (1.1 ml) and the solution was stirred at 80° C. for 3 hours. To the reaction mixture was added ethyl acetate, and the solution was washed with an aqueous solution of sodium hydrogen carbonate and water, then dried (Na2SO4), followed by concentration to dryness. The concentrate was purified by column chromatography on silica gel to give crystals. Recrystallization from ethyl acetate--benzene afforded colorless crystals (1.54 g, 47%), m.p. 163-164° C.

1. washthe solution was washed with an aqueous solution of sodium hydrogen carbonate and water
2. dry with materialdried (Na2SO4)
3. concentrationfollowed by concentration to dryness
4. customThe concentrate was purified by column chromatography on silica gel
5. customto give crystals
6. customRecrystallization from ethyl acetate