Organic compound containing dibenzo six-membered rings and application of organic compound
An organic compound and six-membered ring technology, which is applied to compound materials containing a dibenzo six-membered ring structure as the central skeleton, and the application field in the OLED field, can solve very different problems
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Embodiment 1
[0055] Embodiment 1: the synthesis of intermediate BI:
[0056]
[0057] (1) In a 250ml three-necked flask, under a nitrogen atmosphere, add 0.1mol raw material M, 0.15mol raw material N, 0.3mol sodium tert-butoxide, 1×10 -3 mol Pd 2 (dba) 3 , 1×10 -3 mol P(t-Bu) 3 , 150ml of toluene, heated and refluxed for 24 hours, sampled and plated, the reaction was complete; naturally cooled, filtered, the filtrate was rotary evaporated, and passed through a silica gel column to obtain intermediate L with a HPLC purity of 99.2% and a yield of 50.4%.
[0058] (2) In a 250ml three-necked flask, under a nitrogen atmosphere, add 0.05mol intermediate L, 0.15mol sodium tert-butoxide, 5×10 -4 mol Pd 2 (dba) 3 , 5×10 -4 mol ArNPCy 2 (2-dicyclohexylphosphino-2'-(N,N-dimethylamine)-biphenyl), 150ml 1,4-dioxane, heated to 110°C for 15 hours, sampled and plated, the reaction was complete; Naturally cooled, filtered, the filtrate was rotary evaporated, and passed through a silica gel colu...
Embodiment 2
[0060] Embodiment 2: the synthesis of intermediate BII:
[0061]
[0062] (1) In a 250ml three-necked flask, under a nitrogen atmosphere, add 0.1mol raw material M, 0.15mol raw material N, 0.3mol sodium tert-butoxide, 1×10 -3 mol Pd 2 (dba) 3 , 1×10 -3 mol P(t-Bu) 3 , 150ml of toluene, heated and refluxed for 24 hours, sampled and plated, the reaction was complete; naturally cooled, filtered, the filtrate was rotary evaporated, and passed through a silica gel column to obtain intermediate L with a HPLC purity of 99.2% and a yield of 50.4%.
[0063] (2) In a 250ml three-necked flask, under a nitrogen atmosphere, add 0.05mol intermediate L, 0.15mol sodium tert-butoxide, 5×10 -4 mol Pd 2 (dba) 3 , 5×10 -4 mol ArNPCy 2 (2-dicyclohexylphosphino-2'-(N,N-dimethylamine)-biphenyl), 150ml 1,4-dioxane, heated to 110°C for 15 hours, sampled and plated, the reaction was complete; Naturally cooled, filtered, the filtrate was rotary evaporated, and passed through a silica gel col...
Embodiment 3
[0064] Embodiment 3: the synthesis of intermediate BIII:
[0065]
[0066] (1) In a 250ml three-neck flask, under a nitrogen atmosphere, add 0.1mol raw material O, 0.15mol raw material N, 0.3mol sodium tert-butoxide, 1×10 -3 mol Pd 2 (dba) 3 , 1×10 -3 mol P(t-Bu) 3 , 150ml of toluene, heated and refluxed for 24 hours, sampled and plated, the reaction was complete; natural cooling, filtration, filtrate rotary evaporation, silica gel column, to obtain intermediate P, HPLC purity 99.1%, yield 56.4%.
[0067] (2) In a 250ml three-necked flask, under a nitrogen atmosphere, add 0.05mol of intermediate P, 0.15mol of sodium tert-butoxide, 5×10 -4 mol Pd 2 (dba) 3 , 5×10 -4 mol ArNPCy 2 (2-dicyclohexylphosphino-2'-(N,N-dimethylamine)-biphenyl), 150ml 1,4-dioxane, heated to 110°C for 15 hours, sampled and plated, the reaction was complete; Naturally cooled, filtered, the filtrate was rotary evaporated, and passed through a silica gel column to obtain intermediate BIII with a...
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