反应详情

261 mg (6.87 mmol) lithium aluminium hydride were given to 20 ml tetrahydrofuran (THF) and stirred at room temperature (r.t.) for 20 min. A solution of 1.15 g (4.58 mmol) 6-(3-Trifluoromethyl-phenyl)-pyridine-3-carbaldehyde in 20 ml THF was added drop by drop within 15 min., and the mixture stirred for 3 h. 1.5 ml ice water and 0.6 ml 2 M NaOH were added slowly at 0° C. and stirred continued for 30 min. A formed salt precipitate was isolated by filtration and washed with THF. The combined THF-solutions were evaporated, the residue extracted twice with ethyl acetate, the organic phase dried (sodium sulphate), evaporated, and the obtained material (0.98 g, 85%) used without further purification.

1. stirringthe mixture stirred for 3 h
2. stirringstirred
3. waitcontinued for 30 min
4. customA formed salt precipitate was isolated by filtration
5. washwashed with THF
6. customThe combined THF-solutions were evaporated
7. extractionthe residue extracted twice with ethyl acetate
8. dry with materialthe organic phase dried (sodium sulphate)
9. customevaporated
10. customthe obtained material (0.98 g, 85%) used without further purification