反应详情

With the exclusion of air, 6.0 g (30 mmol) of 4-(pyridin-2-yl)-benzoic acid are suspended at −20° C. in 90 ml of THF, and 9.90 ml (90 mmol) of N-methyl-morpholine and 4.32 ml (33 mmol) of isobutyl chloroformate are added. After 30 min, the mixture is filtered, washed with a small amount of cold THF, and the filtrate is partially concentrated by evaporation; the residue is diluted with methylene chloride, washed with ice-water and cold brine, dried (Na2SO4) and concentrated by evaporation to form the title compound: 1H-NMR (CDCl3) i.a. 8.75 (m, 1H), 8.16 (AB, J=8, 4H), 7.81 (m, 2H), 7.32 (4-line system, J=5, 1H), 4.16 (d, J=7, 2H), 2.10 (9-line system, J=7, 1H), 1.02 (d, J=7, 6H).

1. filtrationthe mixture is filtered
2. washwashed with a small amount of cold THF
3. concentrationthe filtrate is partially concentrated by evaporation
4. additionthe residue is diluted with methylene chloride
5. washwashed with ice-water and cold brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated by evaporation