4-Biphenylylmethyl acrylate synthesis
- Product Name:4-Biphenylylmethyl acrylate
- CAS Number:54140-58-8
- Molecular formula:C16H14O2
- Molecular Weight:238.28
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Yield: 96%
Reaction Conditions:
Stage #1:biphenyl-4-yl methanol with N-benzyl-N,N,N-triethylammonium chloride in toluene
Stage #2:acryloyl chloride with 4-methoxy-phenol at 0 - 40; for 2 h;
Stage #3: with sodium carbonate at 80; for 2 h;Reagent/catalyst;
Steps:
3 Embodiment 3
To the autoclave, 184 g of 4-phenylbenzyl alcohol, 500 g of toluene and 58.5 g of benzyltriethylammonium chloride were added and stirred to dissolve to give a pale yellow transparent solution. The reaction vessel was then placed in a 0-10 ° C in an ice-water bath. The mixture solution of 117.6g acryloyl chloride and 1g p-hydroxyanisole was slowly dropped into the reactor in 1.5h. After the addition of the dissolved solution, the ice water bath was removed and the reaction vessel was placed in 40 ° C warm water Bath continued to react 2h. Then, 400 g of 40% sodium carbonate solution was added dropwise over 1 h. After the addition, the temperature was raised to 80 ° C and the reaction was continued for 2 h to obtain a reaction product solution. The reaction product solution into the water bath, add 200g of deionized water, stirring lOmin after standing lh, release lower wastewater. Then add 200g mass fraction of 10% potassium chloride solution, stirring lOmin after standing lh, release lower waste water. The reaction product solution after water washing was transferred to a reaction kettle, 0.2 g of p-hydroxyanisole was added and the temperature was controlled to 65 ° C. The water-carrying agent was removed under reduced pressure until the content of the water-carrying agent was less than 500 ppm, Yellow transparent 4-phenylbenzyl acrylate.
References:
Zhangjiagang Kangde New Photoelectric Material Co., Ltd;Liu, Yongqiang;Zhang, Qingwei;Ding, Qinghua CN106117054, 2016, A Location in patent:Paragraph 0057; 0058; 00598; 0079
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