反应详情

A mixture of 9-[2-(1-piperidinyl)ethyl]-2,4-di-1-pyrrolidinyl-9H-pyrimido[4,5-b]indole (I, EXAMPLE5, 44 g) and aqueous hydrochloric acid (1M, 107 mL) in ethanol (900 mL) is stirred at 60° until the mixture becomes homogeneous. The mixture is concentrated under reduced pressure in a stream of nitrogen. When the reaction volume reaches approximately half of the original volume, crystallization begins. The mixture is cooled to -10° for 3 hr and the title compound, is isolated by filtration, mp >260°; NMR (CDCl3) 7.88, 7.52, 7.28, 7.13, 4.86, 3.94-3.89, 3.62, 3.45, 3.15 and 2.01-1.96 δ.

1. concentrationThe mixture is concentrated under reduced pressure in a stream of nitrogen
2. customhalf of the original volume, crystallization
3. temperatureThe mixture is cooled to -10° for 3 hr