反应详情

In 46 ml of anhydrous toluene, is dissolved 1.44 g of 6-cyano-2,2-dimethyl-4-(1,2-dihydro-2-oxo-4-(1-phenoxythiocarbonyloxy-4-p-methoxybenzyloxybutyl)-1-pyridinyl}-2H-benzo[b]pyran obtained in Example 45. Then, 0.76 g of 2,2'-azobisisobutyronitrile and 1.35 g of tri-n-butyltin hydride are added and reacted at 100° C. for 15 minutes. After the reaction, the reaction mixture is directly purified by silica gel column chromatography using 3/2 mixture of ethyl acetate/n-hexane as a developing solvent. Thus, 1.03 g of 6-cyano-2,2-dimethyl-4-{1,2-dihydro-2-oxo-4-(4-p-methoxybenzyloxybutyl)-1pyridinyl-}-2H-benzo[b]pyran is obtained.

1. customreacted at 100° C. for 15 minutes
2. customAfter the reaction
3. customthe reaction mixture is directly purified by silica gel column chromatography
4. addition3/2 mixture of ethyl acetate/n-hexane as a developing solvent