反应详情

4M HCl/dioxane (0.609 ml, 2.43 mmol) was added to a solution of (R)-tert-butyl 4-(4-chlorophenyl)-2-methyl-5-(4-(5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)-5-oxopentan-2-ylcarbamate (0.044 g, 0.0812 mmol) in dioxane (1 mL). The reaction mixture was stirred at room temperature for 2 days, after which it was concentrated to dryness. The resulting residue dissolved in minimal MeOH, and the product was triturated by the addition of ether. The solids were isolated by filtration through quantitative membrane filter paper with nitrogen pressure, rinsed with ether, and dried in vacuo to give (R)-4-amino-2-(4-chlorophenyl)-4-methyl-1-(4-(5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)pentan-1-one dihydrochloride (0.035 g, 83.7% yield) as a white powder. LC/MS (APCI+) m/z 442 [M+H]+. 1:1 mixture of diastereomers.

1. concentrationafter which it was concentrated to dryness
2. dissolutionThe resulting residue dissolved in minimal MeOH
3. customthe product was triturated by the addition of ether
4. customThe solids were isolated by filtration through quantitative membrane
5. filtrationfilter paper with nitrogen pressure
6. washrinsed with ether
7. customdried in vacuo