反应详情

温度

55 °C

4-{4-[4-((R)-1-Phenyl-ethylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzyl}-piperazine-1-carboxylic acid tert-butyl ester (1.8 g, 3.5 mmol) is dissolved in 150 mL of dioxane by gentle warming. To this solution is added a solution of 4 N hydrochloric acid in dioxane (Aldrich, Buchs, Switzerland) (5 mL, 20 mmol) and the mixture stirred at 50 to 60° C. for 1 hour. The resulting suspension is diluted with 75 mL of methanol and stirred for 1 additional hour under reflux after which the mixture is cooled and the solvent evaporated. The residue is dissolved in diluted hydrochloric acid and washed with ethyl acetate. The aqueous phase is treated with solid potassium carbonate until basic and evaporated. The residue which contains inorganic salts is purified by flash chromatography using dichloromethane/methanol 7:3 containing 1% conc. ammonia. Pure fractions were taken up in ethyl acetate, washed with water and brine, dried with sodium sulfate and evaporated to give the title compound as a solid; m.p. 240-242° C.; MS-ES+: (M+H)+=413; TLC Rf(dichloromethane/methanol 7:3 containing 1% conc. ammonia) 0.35; HPLC tR=6.86 min.

1. stirringstirred for 1 additional hour
2. temperatureunder reflux after which the mixture
3. temperatureis cooled
4. customthe solvent evaporated
5. dissolutionThe residue is dissolved in diluted hydrochloric acid
6. washwashed with ethyl acetate
7. additionThe aqueous phase is treated with solid potassium carbonate until basic and
8. customevaporated
9. customis purified by flash chromatography
10. washwashed with water and brine
11. dry with materialdried with sodium sulfate
12. customevaporated