1,2-Methylenedioxybenzene CAS 274-09-9

Safrole, also known as safrole, English name Safrole, colorless or light yellow liquid, has the smell of camphor wood, its structural formula is. Soluble in ethanol, miscible with chloroform and ether, insoluble in water and glycerol. The relative density is 1.096, the freezing point is about 11°C, the boiling point is 232-234°C, the refractive index is 1.538, and the flash point is 97°C. Safrole is the main component of many edible natural flavors such as sassafras essential oil, star anise essential oil and camphor oil, accounting for about 80% of sassafras essential oil. Safrole is also found in small amounts in flavors made from nutmeg, Japanese wild ginger, California laurel and other spices exist. Sassafras essential oil is often used as a flavor addition to beer and other liquors. The root bark of the sassafras tree (Sas-safrasalbidum) is also the main ingredient in a popular medicinal tonic tea, sassafras tea. CN201410079934.9 provides a kind of preparation method of safrole, the steps are as follows:

Add piperonyl ring and allyl alcohol to the reactor, then add catalyst Nafion-H, control the temperature to be 15-50°C, and carry out the Friedel-Crafts reaction at a stirring speed of 500-800r/min for 6-10h to obtain a reaction solution;

The amount of piperonyl ring used in the above-mentioned Friedel-Crafts reaction, allyl alcohol, calculated in molar ratio, namely piperonyl ring: allyl alcohol is 30:1; Ratio calculation, that is, catalyst Nafion-H: piperonyl ring is 10:100;

The reaction solution obtained above is filtered, and the obtained filtrate is first washed with saturated sodium bicarbonate solution 2-3 times, then washed with tap water for 2-3 times, dried at room temperature with anhydrous sodium sulfate, and then filtered to remove the anhydrous Sodium sulfate, the filtrate obtained is the piperonyl ring solution of safrole;

Beneficial technical effects of the present invention

The preparation method of safrole of the present invention uses commercially available allyl alcohol and piperonyl ring as raw materials, and under the action of catalyst Nafion-H, obtains safrole through Friedel-Crafts reaction in one step, so the preparation process is simple and suitable for large-scale At the same time, because the piperonyl ring is also used as a solvent in the preparation process, the substances used in the preparation process are few, and the production cost is low.

New ocean jasmine aldehyde is a kind of preparation spice with the scent of flowers with ozone-like top fragrance. It not only has the fragrance of fresh flowers and herbs such as gentle rabbit ear aldehyde, lilac, new mowing grass and cyclamen, etc., but also has fresh melon and watermelon. This kind of fruity green fragrance can be used to reconcile almost all floral notes such as cyclamen, jasmine and rose.

CN201310230531.5 proposes a chemical preparation method of new jasmonaldehyde with easily available raw materials and reasonable process. The preparation method of high-content new jasmine aldehyde of the present invention comprises the steps of:

a) Add 300～380Kg of piperonyl ring and 10～15Kg of boron trifluoride into the enamel reaction kettle by vacuum suction method. After the feeding is completed, nitrogen is introduced to replace the vacuum, and 0.1～15kg of oil-soluble antioxidant is added into the enamel reaction kettle. 1Kg, turn on the mixer and mix evenly;

b) Add 200-280Kg of piperonyl ring to the stirring pot, then add 200-250Kg of 2-methylallyl diacetate to prepare a dropwise mixture;

c) Turn on the chilled water to cool down the enamel reaction kettle. When the temperature of the kettle is lower than 10°C, start adding the mixture of piperonyl ring and 2-methylallyl diacetate dropwise at normal pressure, and control the temperature of the kettle at – 10～15℃, dripping time 4～10 hours;

d) Transfer the reaction product of step c) to a still, and recover it under the conditions of a pressure of -0.01 MPa, a temperature of 60 to 185 °C in the still, a temperature of 60 to 130 °C at the top of the tower, and a reflux ratio of 1:10 to 2:1. Pepper ring, when the temperature at the top of the tower drops and no material is discharged, the temperature of the kettle is lowered, and the recovery of the pepper ring ends;

e) Controlling the pressure in the distillation still to -0.09MPa, the temperature of the still to 120～180℃, the reflux ratio to 4:1～1:8, and the content of the new jasmonaldehyde monoester, the intermediate product of the fractionation reaction, to be 80～95wt%,

f) Enter 100-200Kg of methanol, 50-120Kg of water and 100-150Kg of potassium hydroxide in sequence into the reaction kettle, turn on the mixer and stir evenly, then add 200-300Kg of new jasmonaldehyde monoester; the reaction kettle is slowly heated up to 50-90 ℃, maintain the kettle temperature at 50～90 ℃ and carry out the hydrolysis reaction, and continue to stir for 3～5 hours, lower the temperature to terminate the reaction, and move to the water washing pot and let stand for 30 minutes, separate the lower layer of water and carry out the next batch of hydrolysis;

g) Transfer the reaction product in the water washing pot in step f) to the fractionation kettle, raise the temperature of the fractionation kettle to 50-90° C., and recover methanol at normal pressure. When the temperature at the top of the tower drops and no material is discharged, the recovery of methanol ends;

h) Control the pressure in the fractionation kettle to -0.09MPa, the temperature of the kettle to 120～180℃, and the reflux ratio to be 4:1～1:8 to fractionate crude jasmonaldehyde. , the crude product of Xinyang jasmonaldehyde was fractionated to obtain a finished product with a high content of 98.5wt%.