Hydrochloric Acid → HCID 69932725, compound
Reaction equation
[OH-].[Na+].[C:3]1([OH:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.CN1[CH2:16][CH2:15][CH2:14][C:13]1=O>>[C:3]1([OH:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:3]1([OH:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:3]1([CH:13]=[CH:14][C:15]2[CH:16]=[CH:5][CH:4]=[CH:3][CH:8]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1Participants
Conditions
- Temperature
- 140 °C
Procedure
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).
Workup
- customTo a 2-liter four-necked flask equipped with a thermometer, stirrer and condenser
- customThe solvent was recovered under reduced pressure
- additionthe reaction mixture was charged into 1000 g of ion-exchanged water
- filtrationthe precipitated crystals were filtrated
- washThe crystal was washed with water (1000 g×3 times)
- customdried under reduced pressure for 8 hours at 80° C.
Sources & evidence
- ORD record
- ord-0fbeb0e61ec649cd871b82d721fe91b6
- Source dataset
- uspto-grants-2001_07
- Patent number
- US06255409B1
Reaction notes
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