反应详情

(S)-tert-butyl 2-((S)-1-(4-chlorophenyl)-2-(4-((5R,7R)-7-hydroxy-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)-2-oxoethyl)pyrrolidine-1-carboxylate (0.74 g, 1.331 mmol) was dissolved in dioxane (3 mL) and treated with 4M hydrogen chloride in dioxane (8.317 mL, 33.27 mmol). The mixture was stirred at ambient temperature for 8 hours. The reaction was concentrated in vacuo, re-dissolved and re-concentrated from MeOH three times. Then the residue was re-dissolved in MeOH (3 mL) and added dropwise to stirred Et2O (100 mL). After stirring for 30 minutes, the solid was collected, washed with Et2O, and then air-dried under a blanket of nitrogen. (S)-2-(4-Chlorophenyl)-1-(4-((5R,7R)-7-hydroxy-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)-2-((S)-pyrrolidin-2-yl)ethanone was recovered as a white solid, (0.47 g, 79%). MS (ESI+) [M+H] 456.1/458.1

1. concentrationThe reaction was concentrated in vacuo
2. dissolutionre-dissolved
3. concentrationre-concentrated from MeOH three times
4. dissolutionThen the residue was re-dissolved in MeOH (3 mL)
5. additionadded dropwise
6. stirringto stirred Et2O (100 mL)
7. stirringAfter stirring for 30 minutes
8. customthe solid was collected
9. washwashed with Et2O
10. customair-dried under a blanket of nitrogen
11. custom(S)-2-(4-Chlorophenyl)-1-(4-((5R,7R)-7-hydroxy-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)-2-((S)-pyrrolidin-2-yl)ethanone was recovered as a white solid, (0.47 g, 79%)