反应详情

A mixture of 9-(2-methanesulfonyloxyethyl)-2,4-di-1-pyrrolidinyl-9H-pyrimido[4,5-b]indole (IX, EXAMPLE4, 50 g) and piperidine (200 mL) is heated at reflux for 16 hr. Excess piperidine is removed under reduced pressure and the residue is partitioned between methylene chloride and aqueous sodium bicarbonate. The organic phase is washed with saline, dried over sodium sulfate and concentrated to give the title compound, NMR (CDCl3) 7.88, 7.28, 7.20, 7.10, 4.46-4.40, 3.94-3.90, 3.66-3.62, 2.74-2.68, 2.57, 1.98-1.94, 1.64-1.58 and 1.45 δ.

1. temperatureis heated
2. temperatureat reflux for 16 hr
3. customExcess piperidine is removed under reduced pressure
4. customthe residue is partitioned between methylene chloride and aqueous sodium bicarbonate
5. washThe organic phase is washed with saline
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated