反应详情

Trimethylacetyl chloride (180.9 g, 1.500 mols) was added over 1 h to a mixture of 2-amino-6-bromo-pyridine (264.7 g, 1.530 mols), triethylamine (166.7 g, 1.650 mols) and toluene (1 L, KF=2 mg moisture/L) maintaining the temperature below 50° C. The mixture was aged at 25° C. for 42 h. A solution of 1M aqueous HCl (500 mL) was added and the biphasic mixture was filtered (after agitation for 5 min) through a pad of solka floc (10 g) which was washed with toluene (50 mL). The organic phase was separated from the filtrates and was washed with 1M aqueous HCl (2×500 mL), 2% aqueous NaCl (500 mL) and a mixture of saturated aqueous NaCl (250 mL) and saturated aqueous NaHCO3 (25 mL). The organic phase was dried over MgSO4 (10 g), filtered and evaporated to dryness to provide 380.7 g of crude title compound, which was diluted with toluene to give 1480.8 g of crude solution.

1. temperaturemaintaining the temperature below 50° C
2. filtrationthe biphasic mixture was filtered (after agitation for 5 min) through a pad of solka floc (10 g) which
3. washwas washed with toluene (50 mL)
4. customThe organic phase was separated from the filtrates
5. washwas washed with 1M aqueous HCl (2×500 mL), 2% aqueous NaCl (500 mL)
6. additiona mixture of saturated aqueous NaCl (250 mL) and saturated aqueous NaHCO3 (25 mL)
7. dry with materialThe organic phase was dried over MgSO4 (10 g)
8. filtrationfiltered
9. customevaporated to dryness
10. customto provide 380.7 g of crude title compound, which