反应详情

0.58 g (25.06 mmol) sodium are carefully added to 40 mL n-propanol by several portions. The mixture is stirred until the metal is dissolved completely (ca. 45 min). Then 6.00 g (25.1 mmol) 2-chloro-4-iodo-pyridine are slowly added to the mixture. The mixture is stirred at reflux for 3 h. The reaction is quenched by the addition of some water. The solvent is removed in vacuo and to the residue are added 20 mL DMF/MeOH. The mixture is filtrated and the filtrate is purified by HPLC (MeOH/H2O/NH3).

1. dissolutionis dissolved completely (ca. 45 min)
2. stirringThe mixture is stirred
3. temperatureat reflux for 3 h
4. customThe reaction is quenched by the addition of some water
5. customThe solvent is removed in vacuo and to the residue
6. additionare added 20 mL DMF/MeOH
7. filtrationThe mixture is filtrated
8. customthe filtrate is purified by HPLC (MeOH/H2O/NH3)