反应详情

温度

180 °C

(2-Chloro-9-cyclopentyl-9H-purin-6-yl)-(3,4-dimethoxy-benzyl)-amine (446 mg, 1.15 mmol), 3-hydroxypiperidine hydrochloride (791 mg, 5.75 mmol) and K2CO3 (1.19 mg, 8.63 mmol) were suspended in 2,5-lutidine (10 mL) and the mixture was heated at 180° C. for 4 h. After cooling, CH2Cl2 (50 mL) was added and the solution was extracted with brine (2×15 mL). The organic fraction was dried over MgSO4, filtered and evaporated. The residue was purified by flash chromatography (95:5 CH2Cl2/MeOH) to afford the title compound as an off-white foam (427 mg, %). Anal. RP-HPLC (Phenomenex Jupiter, 5 μ, C18, 300 Å, 4.6×250 mm; 1 mL/min): tR=18.4 min (10-70% MeCN in 0.1% aq CF3COOH over 20 min); tR=16.0 min (35-45% MeCN in 0.1% aq CF3COOH over 20 min); purity>95% (λ=214 nm). DE-MALDI-TOF MS: [M+H]+=453.9 (C24H32N6O3=452.6).

1. temperatureAfter cooling
2. extractionthe solution was extracted with brine (2×15 mL)
3. dry with materialThe organic fraction was dried over MgSO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by flash chromatography (95:5 CH2Cl2/MeOH)