反应详情

0.03 Mole of butyl lithium in hexane as a 15% w/w solution was added dropwise to a stirred, cooled (-10° C.) solution of 5.46 grams (0.03 mole) of 4-benzylideneamino pyridine in 10 milliliters of dry ether. The mixture was allowed to warm to room temperature and then poured onto ice and extracted with methylene chloride. The organic phase was separated and extracted with 2 N hydrochloric acid. The extracts were basified with 2 N sodium hydroxide and extracted into methylene chloride. The resulting methylene chloride solution was dried (MgSO4) and decolourised with charcoal. The solvent was removed and the resulting light oil (5.75 grams) was crystallised and recrystallised from a toluene/petrol 60°-80° C.) mixture affording 2.36 grams of N-([α-phenyl]-n-pentyl)-4-pyridinamine, melting point 118°-8.5°.

1. additionpoured onto ice
2. extractionextracted with methylene chloride
3. customThe organic phase was separated
4. extractionextracted with 2 N hydrochloric acid
5. extractionextracted into methylene chloride
6. dry with materialThe resulting methylene chloride solution was dried (MgSO4)
7. customThe solvent was removed
8. customthe resulting light oil (5.75 grams) was crystallised
9. customrecrystallised from a toluene/petrol 60°-80° C.) mixture