反应详情

2.60 mg (68.44 mmol) lithium aluminium hydride were given to 110 ml tetrahydrofuran (THF) and stirred at room temperature (r. t.) for 20 min. A solution of 11.20 g (34.22 mmol) 6-(2-Fluoro-4-trifluoromethyl-phenyl)-2-methyl-nicotinic acid methyl ester in 110 ml THF was added drop by drop at 0° C. within 15 min., and the mixture stirred for 2 h at 0° C. 140 ml brine were added slowly at 0° C. and stirred continued for 1 h. The mixture was adjusted to pH=5 by slowly addition of conc. HCl. 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) and evaporated. The obtained material (9.69 g, 99%) used without further purification.

1. stirringthe mixture stirred for 2 h at 0° C
2. stirringstirred
3. waitcontinued for 1 h
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 (9.69 g, 99%) used without further purification