2-Propenoic acid 2-([1,1'-biphenyl]-2-yloxy)ethyl ester synthesis
- Product Name:2-Propenoic acid 2-([1,1'-biphenyl]-2-yloxy)ethyl ester
- CAS Number:91442-24-9
- Molecular formula:C17H16O3
- Molecular Weight:268.31
Yield:-
Reaction Conditions:
Stage #1: 2-hydroxyethyl acrylatewith p-toluenesulfonyl chloride;trimethylamine in dichloromethane at 0; for 7 h;
Stage #2: 2-Phenylphenolwith potassium carbonate in acetonitrile at 80;
Steps:
4 Preparative Example 4
To a 3000 ml flask equipped with a cooling pipe and a stirrer, 300 ml of dichloromethane (Sigma-Aldrich) was charged, 200 g of hydroxylethyl acrylate (Shin-Nakamura Chemical Co., Ltd.) and 168 g of trimethylamine were added. After the temperature in the flask was allowed to decrease to 0° C., the solution in which 278 g of p-toluene sulfonyl chloride (Sigma-Aldrich) was dissolved in 500 ml of dichloromethane was drop-wise added for 2 hours while stirring. After stirring for 5 hours again, the remaining solvent was removed by distillation. 300 g of the obtained compound was added to 1000 ml of acetonitrile (Sigma-Aldrich), and 220 g of potassium carbonate (Sigma-Aldrich) and 141 g of 2-phenylphonol (Sigma-Aldrich) were added again, and stirred at 80° C. Then, the remaining solvent and the reaction residues were removed to obtain a compound of formula 8 (molecular weight 296.36) having a purity of 93% as determined by HLPC.
References:
US2017/298164,2017,A1 Location in patent:Paragraph 0122
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