One-step synthesis method of 2, 5-dialkyl furan
A technology of an alkyl furan and a synthesis method, applied in directions such as organic chemistry, can solve problems such as unfavorable large-scale utilization, reduced service life of metal equipment, long synthesis cycle application, etc., and achieves advantages of industrial production and efficiency, and simple post-reaction treatment. The effect of facile, high-efficiency atom-economic synthesis
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Embodiment 1
[0040] Synthesis of 2,5-diethylfuran:
[0041]
[0042] Such as figure 2 As shown, furan (50 mmol, 3.404 g), N,N'-tetramethylethylenediamine (90 mmol, 10.459 g) and 100 mL of anhydrous and oxygen-free tetrahydrofuran (redistillation process of anhydrous and oxygen-free tetrahydrofuran are detailed See figure 1 , is a method well known to those skilled in the art, and will not be described in detail here) into a 250 mL three-necked flask equipped with a constant pressure dropping funnel and a reflux condenser, slightly evacuated, filled with nitrogen, and reciprocated 3 times in sequence. The flask was stirred in an ice-water bath for 0.5 h, and then slowly added dropwise with a n-butyllithium solution in n-hexane (90 mmol, 2.5 mol / L, 36 mL). After the addition was complete, the stirring was continued for 0.5 h under an ice-water bath. Then the mixture was moved to room temperature and warmed to reflux at 66 °C for 4 h. The mixture was cooled to room temperature, then mo...
Embodiment 2
[0045] Synthesis of 2,5-dioctylfuran:
[0046]
[0047] Furan (50 mmol, 3.404 g), N,N'-tetramethylethylenediamine (90 mmol, 10.459 g) and 100 mL of anhydrous and oxygen-free tetrahydrofuran were added to a tank equipped with a constant pressure dropping funnel and a reflux condenser. In a 250 mL three-neck flask, vacuumize slightly, fill with nitrogen, reciprocate 3 times in sequence, and then place it in an ice-water bath and stir for 0.5 h. Slowly add n-butyl lithium in n-hexane solution (90mmol, 2.5 mol / L, 36 mL) dropwise, after the addition is complete, continue stirring for 0.5 h under ice-water bath. The mixture was then moved to room temperature and warmed to reflux at 66 °C for 4 h. Then the mixture was cooled to room temperature, then transferred to an ice-water bath and stirred for 0.5 h. Bromooctane (90 mmol, 17.381 g) was slowly added dropwise. After the addition was complete, it was moved to room temperature and stirred overnight. Added to 100 mL of saturate...
Embodiment 3
[0050] Synthesis of 2,5-Diisooctylfuran:
[0051]
[0052] Add furan (50 mmol, 3.404 g), N,N'-tetramethylethylenediamine (90 mmol, 10.459 g) and 100 mL of anhydrous and oxygen-free tetrahydrofuran into a tank equipped with a constant pressure dropping funnel and a reflux condenser In a 250 mL three-neck flask, vacuumize slightly, fill with nitrogen, reciprocate 3 times in sequence, and then place it in an ice-water bath and stir for 0.5 h. Slowly add n-butyl lithium in n-hexane solution (90mmol, 2.5 mol / L, 36 mL) dropwise, after the addition is complete, continue stirring for 0.5 h under ice-water bath. The mixture was then moved to room temperature and warmed to reflux at 66 °C for 4 h. Then the mixture was cooled to room temperature, then placed in an ice-water bath and stirred for 0.5 h. Bromoisoctane (90 mmol, 17.381 g) was slowly added dropwise. After the addition was complete, it was moved to room temperature and stirred overnight. Added to 100 mL of saturated aque...
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