2,6-Diphenylphenol synthesis
- Product Name:2,6-Diphenylphenol
- CAS Number:2432-11-3
- Molecular formula:C18H14O
- Molecular Weight:246.3
Yield:2432-11-3 99.3%
Reaction Conditions:
with palladium diacetate;dicyclohexylphenylphosphine in water;1,2-dichloro-ethane at 40 - 70; for 3 h;Inert atmosphere;Sealed tube;Suzuki Coupling;Reagent/catalyst;Solvent;Temperature;Concentration;
Steps:
6.1; 6.2; 6.3 Example 6
Example 6(1) under nitrogen at room temperature,A 2 L three-necked flask was charged with 2,6-dichlorophenol (0.9 mol, 146.7 g)0.05 mol of phenylboronic acid, 0.045 mol of palladium acetate,Dicyclohexyl phenyl phosphine 0.0045mol and dichloroethane 790.6g added to the medium, through the dry steady nitrogen flow, the system sealed, stirring up to 40 ;(2) In step (1), 600 g of potassium phosphate aqueous solution (containing 1.8 mol of potassium phosphate) was added dropwise to control the dropping rate to keep the temperature of the system at 40 ° C,Drop Bi system temperature to 70 , keep heating 2h,TLC monitoring no intermediate 2 - chloro - 6 - phenyl phenol remaining to stop the insulation, cooling 40 , standing stratification, separation of water, organic phase;(3) the organic phase washed to neutral, anhydrous sodium sulfate drying, at 90 , vacuum 0.095MPa out of dichloro B Alkyl to give crude 2,6-diphenylphenol with a purity of GC> 98%. Cooled to 0 ° C filtered and dried to give 223.1 g of white needle-like powder.GC: 99.9%, the total yield of 99.3%, the melting point of 101.4 ~ 104.7 .
References:
Yantai Haichuan Chemicals Co., Ltd.;Wang Shulin;Wang Baohua;Gong Zhenshan;Feng Shaoquan;Li Jun;Zhao Feng CN106631708, 2017, A Location in patent:Paragraph 0027; 0028; 0029-0055; 0056; 0057; 0058; 0059
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