反应详情

Heated a reaction mixture of 4-(benzyloxy)-1-(3-fluorobenzyl)pyridin-2(1H)-one (4.83 g, 15.6 mmol) in anhydrous acetonitrile (55 mL) and N-iodosuccinimide (NIS, 3.86 g, 17.1 mmol) under nitrogen atmosphere at 65° C. for 4 h. The reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography (silica gel) using EtOAc/hexanes (1:1 v:v). The appropriate fractions were collected according to ES MS (M+H 436) and washed with Na2SO3 to remove the color impurities. The fractions were concentrated under reduced pressure and dried in vacuo to afford the desired product (6.15 g, 90%) as a light yellow solid.

1. temperatureHeated
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. customthe residue was purified by flash chromatography (silica gel)
4. customThe appropriate fractions were collected
5. washwashed with Na2SO3
6. customto remove the color impurities
7. concentrationThe fractions were concentrated under reduced pressure
8. customdried in vacuo