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ChemicalBook CAS DataBase List m-DCPBA
854952-51-5

m-DCPBA synthesis

10synthesis methods
750573-24-1 Synthesis
9,9'-(5-bromo-1,3-phenylene)bis(9H-carbazole)

750573-24-1
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$45.00/10mg

m-DCPBA

854952-51-5
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Yield:854952-51-5 80%

Reaction Conditions:

Stage #1: 9,9’-(5-bromo-1,3-phenylene)bis(9H-carbazole)with n-butyllithium in tetrahydrofuran at -78; for 3 h;Inert atmosphere;
Stage #2: Triisopropyl borate in tetrahydrofuran at -78; for 2 h;Inert atmosphere;

Steps:



Dissolve 0.018 mol of intermediate 1-1 in 100 ml,In dry THF,After adding the dried 500ml three-necked bottle,Under N2 protection -78 °C reaction for 30min, Slowly add 0.027 mol of n-butyllithiumAfter the end of dropping, the reaction was held at -78°C for 3 hours. Slowly add triisopropyl borate 0.02mol,After the addition was completed, the reaction was held at -78°C for 2 hours.Slowly warm up to room temperature, react overnight, after TLC monitoring reaction is over,The reaction solution was slowly quenched with water, extracted and evaporated to give 0.0144 mol of Intermediate 2-1.The rate of production is 80%.Intermediates 2-2 to 2-4 were synthesized according to the preparation method of the above Intermediate 2-1.

References:

CN107619406,2018,A Location in patent:Sheet 0034-0035