Reaktion #66471

Reaktionsgleichung

(2-chloro-purin-4-yl)-(5-methyl-1H-pyrazol-3-yl)-amine

4-methylpiperidine

Potassium carbonate

→

solid

Ausbeute 90.0%

[2-(4-Methylpiperidin-1-yl)-purin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine

Ausbeute 90.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction mixture heated
2. 2
   Temperaturat reflux overnight
3. 3
   SonstigeThe solvent was evaporated
4. 4
   workup.DISSOLUTIONthe residue dissolved in a mixture EtOH:water (1:3, 4 mL)
5. 5
   FiltrationThe resulting suspension was filtered
6. 6
   Waschenwashed with water (×2)
7. 7
   Waschenrinsed with Et2O (×2)

Vorschrift

To a solution of (2-chloro-purin-4-yl)-(5-methyl-1H-pyrazol-3-yl)-amine (200 mg, 0.80 mmol) was added 4-methylpiperidine (4 mL, 8.01 mmol) and the reaction mixture heated at reflux overnight. The solvent was evaporated and the residue dissolved in a mixture EtOH:water (1:3, 4 mL). Potassium carbonate (57 mg, 0.41 mmol) was added and the mixture was stirred at room temperature for 2 hours. The resulting suspension was filtered, washed with water (×2) and rinsed with Et2O (×2) to afford IV-33 as a white solid (225 mg, 90%): mp>300° C.; 1H NMR (DMSO) δ 0.91 (3H, d), 1.10 (2H, m), 1.65 (3H, m), 2.24 (3H, s), 2.84 (2H, m), 4.60 (2H, m), 6.40 (1H, s), 7.87 (1H, m), 9.37-9.59 (1H, m), 12.03-12.39 (2H, m); IR (solid) 1651, 1612, 1574, 1484, 1446, 1327, 1317, 1255, 1203; MS 313.3 (M+H)+.

Quelle