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ChemicalBook CAS DataBase List 5-(4'-Bromomethyl-1,1'-biphenyl-2-yl)-1-triphenylmethyl-1H-tetrazole
124750-51-2

5-(4'-Bromomethyl-1,1'-biphenyl-2-yl)-1-triphenylmethyl-1H-tetrazole synthesis

13synthesis methods
-

Yield:124750-51-2 95.2%

Reaction Conditions:

with bromine in hexane;water at 69; for 0.433333 h;Irradiation;Flow reactor;Temperature;Solvent;

Steps:

4 Example 4:

The structure of the reaction device is shown in Fig. 1. The reactor 8 is a pipe. The length of the pipe is 50m, the diameter is 2mm, the pipe material is a PTFE pipe, and the light source 6 is a fluorescent lamp.First, turn on the light source 6, turn on the preheating pipe in the inner circulating constant temperature water bath 7 and add 100 mL of water to the receiving tank 10.The reaction temperature is 69° C.; 95.6 g (0.2 mol) of 2′-[(N-trityl)tetrazole]-4-methylbiphenyl and 96.0 g (0.6 mol)) Bromine was dissolved in 240 mL of n-hexane and stored in liquid storage tank a1 and liquid storage tank b2, respectively.Turn on infusion pump a4 and infusion pump b5 to regulate the flow,The 2′-[(N-trityl)tetrazole]-4-methylbiphenyl and bromine were continuously fed into the high-efficiency mixer 3 and mixed.Then enter into the light pipe in the internal circulation constant temperature water bath 7 and the reaction time is 26 min.Then directly enter the receiving tank 10, and add 62.4 g of sodium bisulfite to the receiving tank 10 to quench and separate the liquid.The organic phase is concentrated under reduced pressure to remove the solvent, recrystallized by adding ethanol, and suction filtered.After the filter cake was dried, 106.1 g of 2′-[(N-trityl)tetrazole]-4-bromomethylbiphenyl was obtained as a pure product. The yield was 95.2%, and the HPLC purity was 99.3%.

References:

CN107935956,2018,A Location in patent:Paragraph 0022-0029

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