A method for synthesizing carvacrol with dipentene dioxide
A technology of dipentene dioxide and carvacrol, which is applied in the chemical industry, can solve the problems of limited application, environmental pollution, aluminum salt and iron salt solid waste generation, etc., and achieves a simple method, strong operability, and reduction of three industrial wastes Effect
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Embodiment 1
[0029] (1) α,α,6-Trimethyl-7-oxabicyclo[4.1.0]heptane-3-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2] Synthesis of Octan-6-ol:
[0030] In the reactor, add 600g ethanol, 600g content and be 85% dipentene dioxide, stir and mix evenly, add 84.5gNaBH in addition 4 Dissolve in 246g of water, heat the mixed solution in the reactor to 30°C, then start to add NaBH dropwise to the reactor 4 Aqueous solution, dropping time is 3h, then keep warm at 30℃ for 4h, the reaction is completed, and α,α,6-trimethyl-7-oxabicyclo[4.1.0]heptane-3-methanol and 1,3 ,3-trimethyl-2-oxabicyclo[2.2.2]octan-6-ol, and by-products 1-methyl-4-(2-methyl-epoxy)-cyclohexanol and 1, 8-terpene diol, the conversion rate is 95%, the selectivity is 83%, the reaction solution is washed to neutrality, and 395g α,α,6-trimethyl-7-oxabicyclo[4.1 .0]heptane-3-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2]octan-6-ol, yield: 76.5%;
[0031] (2) Synthesis of isodihydrocarvone:
[0032] To 395g α,α,6-trimethyl-7-oxa...
Embodiment 2
[0037] (1) α,α,6-Trimethyl-7-oxabicyclo[4.1.0]heptane-3-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2] Synthesis of Octan-6-ol:
[0038] In the reactor, add 600g ethanol, 600g content and be 85% dipentene dioxide, stir and mix evenly, add 51.9gNaBH in addition 4 Dissolve in 246g of water, cool down the mixed solution in the reactor to 0°C, then start to add NaBH dropwise to the reactor 4 Aqueous solution, dropping time is 3h, then keep warm at 0°C for 24h, after the reaction is over, α,α,6-trimethyl-7-oxabicyclo[4.1.0]heptane-3-methanol and 1, 3,3-Trimethyl-2-oxabicyclo[2.2.2]octan-6-ol, and by-products 1-methyl-4-(2-methyl-epoxy)-cyclohexanol and 1 ,8-Terpene diol, the conversion rate is 95%, the selectivity is 87%, the temperature is low, the selectivity is high, the reaction solution is washed to neutral, and 406g of α,α,6-trimethyl -7-oxabicyclo[4.1.0]heptane-3-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2]octan-6-ol, yield: 78.6 %;.
[0039] (2) Synthesis of isod...
Embodiment 3
[0044] (1) α,α,6-Trimethyl-7-oxabicyclo[4.1.0]heptane-3-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2] Synthesis of Octan-6-ol:
[0045] In the reactor, add 600g ethanol, 600g content and be 85% dipentene dioxide, stir and mix evenly, add 115.5gNaBH in addition 4 Dissolve in 246g of water, heat the mixed solution in the reactor to 50°C, then start to add NaBH dropwise to the reactor 4 Aqueous solution, dropping time is 3h, then keep warm at 50°C for 2h, after the reaction is over, α,α,6-trimethyl-7-oxabicyclo[4.1.0]heptane-3-methanol and 1, 3,3-Trimethyl-2-oxabicyclo[2.2.2]octan-6-ol, and by-products 1-methyl-4-(2-methyl-epoxy)-cyclohexanol and 1 , 8-terpene diol, the conversion rate is 95%, the selectivity is 79%, the reaction solution is washed to neutral, and 372g α,α,6-trimethyl-7-oxabicyclo[ 4.1.0] Heptane-3-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2]octan-6-ol, yield: 72%;
[0046] (2) Synthesis of isodihydrocarvone:
[0047] To 372g α,α,6-trimethyl-7-oxabicy...
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