Hydrochloric Acid → HCID 69932725, compound

Participants

Reaction Conditions

Reaction Steps

To a 2-liter four-necked flask equipped with a thermometer, stirrer and condenser were added 245.2 g of 48.3% aqueous sodium hydroxide solution and 552 g of N-methylpyrrolidone, and the inner atmosphere was replaced by nitrogen. Under nitrogen flow, the temperature of the solution was raised to 140° C. To this, was added dropwise 225.6 g of the phenol intermediate obtained in Synthetic Example 1 and 676 g of N-methylpyrrolidone solution at 140° C. for 1.5 hours and kept at that temperature for 2 hours. Then, the reaction mixture was cooled to 60° C. and neutralized with 226 g of concentrated hydrochloric acid. The solvent was recovered under reduced pressure, the reaction mixture was charged into 1000 g of ion-exchanged water, and the precipitated crystals were filtrated. The crystal was washed with water (1000 g×3 times) and dried under reduced pressure for 8 hours at 80° C., to obtain 208 g of ayellow crystal (stilbene bisphenol).

Provenance & Evidence