Simple preparation method of 9-hydroxyfluorene-9-carboxylate compound
A technology of ester compound and hydroxyfluorene, applied in the field of organic synthesis, can solve problems such as difficulty in obtaining raw materials, and achieve the effects of less reaction by-products, alleviating the pressure on the environment, and less waste discharge
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[0038] Example 1
[0039] Preparation of 9-ethyl-2-methyl-9-hydroxy-6,8-dimethyl-9H-fluorene-2,9-dicarboxylate:
[0040] Preparation of 9-ethyl-2-methyl-9-hydroxy-6,8 using ethyl 2-(2,4-dimethylphenyl)-2-oxoacetate and methyl 4-iodobenzoate as raw materials -Dimethyl-9H-fluorene-2,9-dicarboxylate, the chemical reaction formula is as follows:
[0041]
[0042] Specific steps are as follows:
[0043] Add palladium acetate (Pd(OAc) to the closed pressure tube 2 ) 4.49 mg (0.02 mmol), 2-(2,4-dimethylphenyl)-2-oxoacetate 41.2 mg (0.2 mmol), methyl 4-iodobenzoate 131.0 mg (0.5 mmol), Silver trifluoroacetate (AgTFA) 88.4mg (0.4mmol), trifluoroacetic acid (TFA) 136.8mg (1.2mmol) and 2-fluoro-5-trifluoromethylaniline 14.3mg (0.08mmol), 1.8mL hexafluoroiso Propanol, 0.2mL anhydrous acetic acid, put the reaction solution in a heater at 100°C and stir for 48 hours. The pass specification is F-254 TLC plate tracking, the reaction raw material no longer consumes less, the product no longer incre...
Example Embodiment
[0045] Example 2
[0046] Preparation of 9-hydroxyfluorene-9-carboxylic acid ester compound is 9-hydroxy-6,8-dimethyl-9H-fluorene-2,9-dicarboxylic acid diethyl ester:
[0047] Preparation of 9-hydroxy-6,8-dimethyl-9H-fluorene-2 using ethyl 2-(2,4-dimethylphenyl)-2-oxoacetate and ethyl 4-iodobenzoate as raw materials ,Diethyl 9-dicarboxylate, the chemical reaction formula is as follows:
[0048]
[0049] Specific steps are as follows:
[0050] Add 4.49mg (0.02mmol) of palladium acetate, 41.2mg (0.2mmol) of ethyl 2,4-dimethylbenzoate and 138.0mg (0.5mmol) of ethyl 4-iodobenzoate in the airtight pressure tube. ), silver trifluoroacetate (AgTFA) 88.4mg (0.4mmol), trifluoroacetic acid 136.8mg (1.2mmol) and 2-fluoro-5-trifluoromethylaniline 14.3mg (0.08mmol), 1.8mL hexafluoroisopropyl Alcohol, 0.2mL of anhydrous acetic acid, put the reaction solution in a heater at 100°C and stir for 48 hours. The pass specification is F-254 TLC plate tracking, the reaction raw material no longer consu...
Example Embodiment
[0052] Example 3
[0053] Preparation of 9-hydroxyfluorene-9-carboxylic acid ester compound is 9-hydroxy-1,3-dimethyl-5-nitro-9H-fluorene-9-carboxylic acid ethyl ester:
[0054] Preparation of 9-hydroxy-1,3-dimethyl-5-nitro-9H- with 2-(2,4-dimethylphenyl)-2-oxoacetate and o-nitroiodobenzene as raw materials The chemical reaction formula of fluorene-9-carboxylic acid ethyl ester is as follows:
[0055]
[0056] Specific steps are as follows:
[0057] Add 4.49mg (0.02mmol) of palladium acetate, 41.2mg (0.2mmol) of ethyl 2-(2,4-dimethylphenyl)-2-oxoacetate, and 124.5 of o-nitroiodobenzene into the airtight pressure tube. mg (0.5 mmol), 88.4 mg (0.4 mmol) of silver trifluoroacetate (AgTFA), 136.8 mg (1.2 mmol) of trifluoroacetic acid and 14.3 mg (0.08 mmol) of 2-fluoro-5-trifluoromethylaniline, 1.8 mL Hexafluoroisopropanol, 0.2mL of anhydrous acetic acid, put the reaction solution in a heater at 100°C and stir for 48 hours. The passing specification is F-254 TLC plate tracking, the rea...
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