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The Synthetic Technology of 2-Biphenyl Methanol
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A technology for the synthesis of biphenylmethanol and its synthesis technology, which is applied in the field of synthesis of novel 2-biphenylmethanol, can solve the problems of little redevelopment and utilization, long residual effect period, etc., achieve good economic and social benefits, low cost, Environmentally friendly effect
Active Publication Date: 2021-01-29
浦拉司科技(上海)有限责任公司
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It has the characteristics of contact killing and stomach poisoning, no systemic and fumigation effects, wide insecticidal spectrum, rapid action, no movement in the soil, relatively safe to the environment, and long residual effect period. The intermediates of insecticides have an annual production capacity of more than 1,000 tons. At present, the mainstream synthesis method of biphenyl alcohol will produce some by-products of 2-methylbiphenyl. After the author's inquiry, these by-products of 2-methylbiphenyl Generally, it can only be purified to about 90%, and it can rarely be developed and utilized. It will have very good economic and social benefits by converting 2-methylbiphenyl with a content of about 90% into 2-biphenylmethanol.
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Embodiment 1
[0026] Embodiment 1. Preparation of raw materials, reagents and equipment
[0027] 2-Methylbiphenyl (90%, GC), Yancheng Kefeite Biochemical Technology Co., Ltd.; Azobisisobutyronitrile, Shanghai Sinopharm Chemical Reagent Co., Ltd.; Chlorine (self-made); Manganese dioxide, Shanghai Sinopharm Chemicals Reagent Co., Ltd.; concentrated hydrochloric acid, Shanghai Sinopharm Chemical Reagent Co., Ltd.; N,N-dimethylformamide (DMF), Shanghai Wohua Chemical Co., Ltd.; PEG-400, Shanghai Sinopharm Chemical Reagent Co., Ltd.; methanol, Shanghai Wohua Chemical Co., Ltd.; Potassium borohydride, Shandong Guobang Pharmaceutical Co., Ltd.; Toluene, Shanghai Sinopharm Chemical Reagent Co., Ltd. Melting point was determined by capillary method, FA2004B electronic balance, Agilent 7820 GC chromatograph; 1HNMR nuclear magnetic resonance instrument was BRUKER AM-400 (400MHz), TMS was the internal standard.
Embodiment 2
[0028] The synthesis of embodiment 2.2-chloromethyl biphenyl
[0029] Heat 2-methylbiphenyl (100g, 0.594mol) and azobisisobutyronitrile (1g) to 130°C, then slowly introduce chlorine gas, control the temperature at about 130°C and react with chlorine for 20 hours, monitor the reaction by GC , 2-methylbiphenyl less than 5% is the end of the reaction. After the reaction, cool and set aside.
Embodiment 3
[0030] The preparation of the mixture of embodiment 3.2-biphenylcarbinol and 2-biphenylformaldehyde
[0031] Add 400 g of water and 40 g of DMF to the reaction solution in the previous step, then raise the temperature to reflux, and react at reflux for 12 hours. The reaction is detected by GC. If the raw material is less than 1%, it is the end of the reaction. Cool down to 50°C, separate the lower organic phase, and set aside.
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Abstract
The invention relates to the technical field of synthesis of liquid crystal material intermediate materials, in particular to a synthesis process of novel 2-biphenylmethanol. In the invention, 2-methylbiphenyl is first chlorinated into 2-chloromethylbiphenyl, and then hydrolyzed into 2-biphenylmethanol. The monochlorinated intermediate and dichlorointermediate produced in the synthesis process are directly hydrolyzed into 2-biphenylmethanol and 2-biphenylcarbaldehyde without separation, and then the mixture is passed through potassium borohydride to remove 2- Biphenyl formaldehyde is reduced to 2-biphenylmethanol, and then refined to obtain the finished product of 2-biphenylmethanol. The synthesis process has the characteristics of easy-to-obtain raw materials, low cost, simple process operation, environmental friendliness, good product quality and high yield.
Description
technical field [0001] The invention relates to the technical field of synthesis of liquid crystal material intermediate materials, in particular to a synthesis process of novel 2-biphenylmethanol. Background technique [0002] Display technology is one of the necessary technologies for people to obtain massive amounts of information every day in the information technology age. Liquid crystal display (LCD) has gradually replaced traditional diode display (CRT) and has been widely used due to its advantages of portability, environmental protection and low power consumption, and has become the current mainstream display mode. Liquid crystal materials are also developing rapidly with the development of LCD devices, and various liquid crystal material compounds are continuously developed. As a liquid crystal material intermediate, 2-biphenylcarbinol has an increasing demand. The synthesis process of 2-biphenylmethanol with simple operation and high product quality will be the k...
Claims
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