反应详情

温度

80 °C

795 mg (5.0 mmol) of 2,6-difluoro-nicotinic acid were dissolved in thionyl chloride (15 ml) and the solution was heated for 2 h at 80° C. Concentration in vacuo was then carried out and the residue was taken up in dioxane (15 ml). 566 mg (5.0 mmol) of thiophen-2-yl-methanamine were then added and the mixture was stirred for 1 h at RT. Concentration in vacuo was then carried out and the residue was taken up in EA, washed with water, a sat. aq. Na2CO3 sol., water again and brine, dried over Na2SO4, filtered and concentrated in vacuo. CC (hexane/EA 7:3) of the residue yielded 605 mg (2.4 mmol, 48%) of 2,6-difluoro-N-(thiophen-2-ylmethyl)nicotinamide.

1. concentrationConcentration in vacuo
2. concentrationConcentration in vacuo
3. washwashed with water
4. dry with materiala sat. aq. Na2CO3 sol., water again and brine, dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo