Megastigmatrienone synthesis method
A technique for the synthesis of macrostigmatrienone and its synthesis method, which is applied in the field of synthesis of macrostigmatrienone, can solve problems such as increased production costs, and achieve the effects of low environmental pollution, strong industrial operability, and mild reaction conditions
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Embodiment 1
[0018] Dissolve 23.6g of α-ionol acetate in 70ml of acetonitrile, add 13g of 70% tert-butyl hydroperoxide, add 1.34g of periodic acid under stirring at -5°C, and react for 8 hours. Separate the organic phase, wash the organic phase with water, and distill off the organic solvent to obtain 21.2 g of 3-oxo-α-ionol acetate.
[0019] The obtained 3-oxo-α-ionol acetate was dissolved in 60 ml of acetone, 0.4 g of sulfuric acid was added, and the mixture was refluxed for 5 hours. Evaporate off acetone and redissolve with ethyl acetate. Wash the organic phase with water to neutrality, and then distill off the organic solvent to obtain the crude macrostigmatrienone. The crude macrostigmatrienone was subjected to vacuum distillation, and the fractions at 86°C-120°C / 7-9mbar were collected to obtain 13.2 g macrostigmatrienone. The purity of macrostigmatrienone detected by GC-MS is 72.3%.
Embodiment 2
[0021] Dissolve 23.6g of α-ionol acetate in 70ml of ethyl acetate, add 10g of 70% tert-butyl hydroperoxide, add 1.73g of periodic acid under stirring at -10°C, and react for 8 hours. The organic phase was separated, washed with water, and the solvent was distilled off to obtain 19.6 g of 3-oxo-α-ionol acetate.
[0022] The obtained 3-oxo-α-ionol acetate was dissolved in 60 ml of acetone, 0.4 g of sulfuric acid was added, and the mixture was refluxed for 15 hours. Evaporate off acetone and redissolve with ethyl acetate. Wash the organic phase with water to neutrality, and then distill off the organic solvent to obtain the crude macrostigmatrienone. The crude macrostigmatrienone was subjected to vacuum distillation, and the fraction at 86°C-120°C / 7-9mbar was collected to obtain 12.27 g macrostigmatrienone. The purity of macrostigmatrienone detected by GC-MS is 73%.
Embodiment 3
[0024] Dissolve 23.6g of α-ionol acetate in 70ml of petroleum ether, add 13g of 70% tert-butyl hydroperoxide, add 1.92g of periodic acid under stirring at 15°C, and react for 8 hours. The organic phase was separated, washed with water, and the solvent was distilled off to obtain 15 g of 3-oxo-α-ionol acetate.
[0025] The obtained 3-oxo-α-ionol acetate was dissolved in 45 ml of acetone, 0.3 g of sulfuric acid was added, and the mixture was refluxed for 30 hours. Evaporate off acetone and redissolve with ethyl acetate. Wash the organic phase with water to neutrality, and then distill off the organic solvent to obtain the crude macrostigmatrienone. The crude macrostigmatrienone was subjected to vacuum distillation, and the fraction at 86°C-120°C / 7-9mbar was collected to obtain 10.15 g macrostigmatrienone. The purity of macrostigmatrienone detected by GC-MS is 62%.
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