Method for preparing 1, 5-hexadiene
A technology of hexadiene and metal, applied in the field of preparation of 1,5-hexadiene, which can solve problems such as the inability to obtain C products
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Embodiment 1
[0039] In the reaction kettle, add 1mmol glycerin, 0.01mmol ammonium perrhenate, 1.5mmol triphenylphosphine, 20mL toluene, replace with nitrogen, and react at 180°C for 18h. Combined with qualitative analysis. The 1,5-hexadiene yield was 28%. Wherein the calculation formula of 1,5-hexadiene yield is as follows:
[0040]
[0041] The formula for calculating the yield of 1,5-hexadiene in subsequent examples is the same as the formula above.
[0042] Among them, the qualitative analysis adopts Agilent 7890A GC / 5975C MS gas chromatography-mass spectrometry, HP-5MS capillary column (30.0mⅹ0.25mmⅹ0.25μm), the detector is a hydrogen flame ionization detector (FID), and the electron ion source (EI): 70eV. Temperature program: 80°C (2min), 20°C·min -1 Rise to 260°C, 260°C (9min). Quantitative analysis uses Agilent 7890A GC gas phase, DB-225MS capillary column (30.0mⅹ0.25mmⅹ0.25μm).
Embodiment 2
[0044] In the reaction kettle, add 1mmol glycerin, 0.01mmol rhenium heptoxide, 1.5mmol triphenylphosphine, 20mL toluene, replace with nitrogen, and react at 180°C for 18h. Combined with qualitative analysis. The gas-phase internal standard method was used for quantification, and the yield of 1,5-hexadiene was 33%.
Embodiment 3
[0046] In the reaction kettle, add 1mmol glycerin, 0.01mmol methyl rhenium trioxide, 1.5mmol triphenylphosphine, 20mL toluene, replace with argon, and react at 160°C for 18h. - Qualitative analysis by mass spectrometry. The gas-phase internal standard method was used for quantification, and the yield of 1,5-hexadiene was 20%.
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