反应详情

A mixture of 9-t-butyl-2,4-di-1-pyrrolidinyl-9H-pyrimido[4,5-b]indole (XII, EXAMPLE 25, 4.0 g) and 100 mL of trifluoroacetic acid is heated at reflux for 2 hr. Approximately one-half of the trifluoroacetic acid is removed by distillation. The reaction mixture is then cooled to 0°, made basic with 25% aqueous sodium hydroxide and extracted with methylene chloride. The combined organic phases are washed with saline, dried over anhydrous sodium sulfate and concentrated. Chromatography (silica gel, 5% ethyl acetate/methylene chloride) gives the title compound, NMR (CDCl3) 7.89, 7.86, 7.26-7.09, 3.95, 3.67 and 2.01-1.95 δ.

1. temperatureis heated
2. temperatureat reflux for 2 hr
3. customApproximately one-half of the trifluoroacetic acid is removed by distillation
4. temperatureThe reaction mixture is then cooled to 0°
5. extractionextracted with methylene chloride
6. washThe combined organic phases are washed with saline
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated