Compounds with 5H-dibenzo[a,d]cycloheptene as cores and application of compounds
A technology of dibenzocycloheptene and benzocycloheptene, which is applied in the preparation of amino compounds, the preparation of organic compounds, organic chemistry, etc., can solve different problems, maintain the stability of the film layer, improve the current efficiency and The effect of life and efficiency improvement
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Embodiment 1
[0050] Example 1: Intermediate B (i.e. H-R 1 , H-R 2 )Synthesis:
[0051]
[0052] Weigh raw material O and raw material P and dissolve with toluene, then add Pd 2 (dba) 3 , P(Ph) 3 and sodium tert-butoxide; under an inert atmosphere, react the mixed solution of the above reactants at a reaction temperature of 90 to 110 ° C for 10 to 24 hours, cool the reaction solution, filter the reaction solution, rotate the filtrate, and pass it through a silica gel column to obtain the target product; The molar ratio of the raw material O to the raw material P is 1:1.0~1.5; Pd 2 (dba) 3 The molar ratio to raw material O is 0.006-0.02:1, and the molar ratio of sodium tert-butoxide to raw material P is 2.0-3.0:1; P(Ph) 3 The molar ratio to raw material O is 2.0~3.0:1;
[0053] Take the synthesis of intermediate B1 as an example:
[0054]
[0055] In a 250ml three-necked flask, under the protection of nitrogen, add 0.01mol aniline, 0.012mol bromobenzene, 150ml toluene, stir and...
Embodiment 2
[0060] Example 2: Synthesis of Intermediate AI and Intermediate AII:
[0061]
[0062] 250ml four-necked bottle, under nitrogen atmosphere, add 0.05mol Br-Ar 1 -Br and 1.2g of Mg powder (0.05mol), 60ml of tetrahydrofuran, heated to reflux for 4 hours, the reaction was complete, and Grignard reagent was generated; 10.3g of dibenzocyclohepten-5-one (0.05mol) was dissolved in 50mL of tetrahydrofuran, dropwise Add the above Grignard reagent, react at 60°C for 24 hours, a large amount of white Grignard salt precipitates, add saturated NHCl 4 The solution was until the precipitation disappeared, and the grit salt was converted into tertiary alcohol; after the reaction was completed, it was extracted with 100 ml of ether, the extract was dried with anhydrous sodium sulfate, and the solution was rotary evaporated to remove the solvent until no fraction was obtained to obtain a crude product of tertiary alcohol. The crude product of tertiary alcohol was The mixed solvent of petrole...
Embodiment 3
[0068] Example 3: Synthesis of Compound 2:
[0069]
[0070] In a 250ml three-necked flask, under the protection of nitrogen, add 0.01mol of Intermediate A2, 0.012mol of Intermediate B1, and 150ml of toluene, stir and mix, and then add 5×10 -5 molPd 2 (dba) 3 , 5×10 -5 mol P(t-Bu) 3 , 0.03mol sodium tert-butoxide, heated to 105 ℃, refluxed for 24 hours, sampling point plate, showed that no bromide remained, the reaction was complete; naturally cooled to room temperature, filtered, the filtrate was rotary evaporated to no fraction, passed through a neutral silica gel column , the target product was obtained, the HPLC purity was 98.8%, and the yield was 76.5%. Elemental analysis structure (molecular formula C 45 H 33 N): Theoretical C, 91.96; H, 5.66; N, 2.38; Tested C, 91.98; H, 5.65; N, 2.37. HPLC-MS: The molecular weight of the material is 587.77, and the measured molecular weight is 587.49.
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