A method for synthesizing ethyl 2,2-difluorohexanoate
A technology of ethyl difluorohexanoate and ethyl bromodifluoroacetate is applied in the field of synthesis and separation of organic compounds, can solve problems such as high price of photocatalysts, achieve low solvent quality requirements, avoid metal residues, and mild reaction conditions Effect
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Embodiment 1
[0030] In a 100ml reaction tube, add diphenyl disulfide (109mg, 0.5mmol) and 2,6-dimethyl-1,4-dihydro-3,5-diethylpyridinedicarboxylate (5.06g, 20mmol ), on the N2 line, after replacing the air in the tube with nitrogen, under nitrogen conditions, butene n-hexane solution (about 15ml of 10% n-hexane solution, 30mmol) and ethyl bromodifluoroacetate (2.03g10mmol), then add 30 mL of dichloromethane. Put the reaction solution under a blue LED lamp or a white energy-saving lamp for 48 hours, then spin dry the solvent with a rotary evaporator, and add petroleum ether (boiling range 30-60°C) to dissolve. Using column chromatography technology with 300-400 mesh silica gel as the stationary phase, wet loading and elution with petroleum ether (boiling range 30-60°C) as the eluent, GC-MS detects the product band, and collects The chromatographic solution was spin-dried to obtain the product ethyl 2,2-difluorohexanoate (780 mg, yield 43%).
[0031] product in deuterated chloroform 1 H N...
Embodiment 2
[0033] Synthetic C 14 h 18 f 2 o 3 :
[0034] In a 10ml transparent reaction test tube, add diphenyl disulfide (2.2mg, 0.01mmol) and 2,6-dimethyl-1,4-dihydro-3,5-pyridinedicarboxylic acid diethyl ester (101.2mg ,0.4mmol), placed in the glove box, replaced with nitrogen, sealed the mouth of the bottle with a polytetrafluoroethylene inner village gasket, took it out from the glove box, and added p-methoxystyrene ( 29.6mg, 0.2mmol) and ethyl bromodifluoroacetate (81.2mg, 0.4mmol), and then added 2mL of acetonitrile. The reaction is easily placed under a blue LED lamp or a white energy-saving lamp for 12-48 hours, and then the solvent is spin-dried by a rotary evaporator, and dissolved by adding n-hexane. Using column chromatography technology with 300-400 mesh silica gel as the stationary phase, wet loading, elution with n-hexane as the eluent, GC-MS detection of the eluent, and spinning the collected chromatographic solution to dryness, The product 1 (24.0 mg, yield 44%) w...
Embodiment 3
[0036] Synthetic C 14 h 18 f 2 o 2 :
[0037] In a 10ml transparent reaction test tube, add diphenyl disulfide (2.2mg, 0.01mmol) and 2,6-dimethyl-1,4-dihydro-3,5-pyridinedicarboxylic acid diethyl ester (101.2mg ,0.4mmol), placed in the glove box, replaced with nitrogen, sealed the mouth of the bottle with a polytetrafluoroethylene inner village gasket, took it out from the glove box, added styrenebutene (29.6mg, 0.2mmol) and ethyl bromodifluoroacetate (81.2mg, 0.4mmol), and then added 2mL of acetonitrile. The reaction is easily placed under a blue LED lamp or a white energy-saving lamp for 12-48 hours, and then the solvent is spin-dried by a rotary evaporator, and dissolved by adding n-hexane. Using a column chromatography technique using 300-400 mesh silica gel as a stationary phase, wet loading, eluting with n-hexane as an eluent, detecting product bands by GC-MS, and spinning the collected chromatographic solution to dryness, that is Product 2 (33.3 mg, yield 65%) cou...
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