反应详情

A stirred solution, under N2, of 8.7 g of 1,2-dihydro-6-phenylindolo[1,7-ab][1,5]benzodiazepine in 125 ml of xylene is heated to 100° C. when 7.34 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) is added in one portion. The mixture is brought to reflux and kept there for 3.0 hours. After cooling to room temperature, the liquid is filtered and the residue remaining in the flask is rinsed with xylene. The xylene filtrate is concentrated to an oil. This oil is dissolved in ethanol, and the solution is allowed to cool at 0° C. The crystals so obtained are filtered, washed with a little ethanol, then dried to yield 6-phenylindolo[1,7-ab][1,5]benzodiazepine, m.p. 128°-136° C.

1. additionis added in one portion
2. temperatureto reflux
3. filtrationthe liquid is filtered
4. washis rinsed with xylene
5. concentrationThe xylene filtrate is concentrated to an oil
6. dissolutionThis oil is dissolved in ethanol
7. temperatureto cool at 0° C
8. customThe crystals so obtained
9. filtrationare filtered
10. washwashed with a little ethanol
11. customdried