反应详情

At RT, 51 g of sodium methoxide (953 mmol, 1.05 equivalents) were initially charged in 1000 ml of methanol, 100 g of 2-amino-3-hydroxypyridine (908 mmol, 1 equivalent) were added and the mixture was stirred at RT for 15 min. The reaction mixture was concentrated under reduced pressure, the residue was taken up in 2500 ml of DMSO and 197 g of 2,6-difluorobenzyl bromide (953 mmol, 1.05 equivalents) were added. After 4 h at RT, the reaction mixture was poured into 20 l of water and stirred for 15 min, and the solid was filtered off. The solid was washed with 1 l of water, 100 ml of isopropanol and 500 ml of petroleum ether and dried under high vacuum. This gave 171 g of the title compound (78% of theory).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. waitAfter 4 h at RT
3. stirringstirred for 15 min
4. filtrationthe solid was filtered off
5. washThe solid was washed with 1 l of water, 100 ml of isopropanol and 500 ml of petroleum ether
6. customdried under high vacuum