反应详情

温度

100 °C

A mixture of 1-(6-chloro-2-pyridinyl)piperazine (6.0 g) and NaOMe (16.42 g) in DMF (25 mL,) was heated at 100° C. under nitrogen atmosphere for 20 h. The excess DMF was then removed under reduced pressure. Water (5 mL) was added to the residue and the mixture extracted with CH2Cl2. The combined organic layers were washed with sat. NaCl solution, dried with anhydrous MgSO4, filtered and concentrated under reduced pressure. Silica gel chromatography (CH2Cl2 /MeOH; 98:2) of the concentrate yielded the 4-(6-methoxy-2-pyridinyl)1-piperazinecarboxaldehyde (5.13 g; 81%).

1. customThe excess DMF was then removed under reduced pressure
2. additionWater (5 mL) was added to the residue
3. extractionthe mixture extracted with CH2Cl2
4. washThe combined organic layers were washed with sat. NaCl solution
5. dry with materialdried with anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure