Toluene → HCID 12080910, compound

Participants

Reaction Steps

Into a 2 liter four-necked flask equipped with a thermometer, a stirrer and a Dean-Stark distillation apparatus, 133.24 g (0.63 moles) of dimethyl 5-hydroxyisophthalate, 107.33 g (0.76 moles) of 4-fluoronitrobenzene, 760 ml of N,N-dimethylformamide and 190 ml of toluene were placed, and the resultant mixture was stirred at 165° C. for 4 hours while water formed by the reaction was removed as an azeotrope with toluene. After the reaction fluid was cooled, the reaction fluid was added into 3 liters of ion-exchanged water, and the product was precipitated. The precipitated product was separated by filtration and washed with ion-exchanged water and ethanol. The obtained light yellow solid substance was dried at 50° C. for 1 day under a reduced pressure, and 142.01 g of the first intermediate compound was obtained (the yield: 68%).

Provenance & Evidence