Process for preparing dihydro-safrole by catalysis hydrogenation

A technology of catalytic hydrogenation of safrole, applied in the direction of organic chemistry, can solve the problems of large amount of solvent, low yield, low hydrogenation rate of dihydrosafrole, etc.

Inactive Publication Date: 2004-12-29
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the defects that the hydrogenation rate of the product dihydrosafrole is low in the process of preparing dihydrosafrole in the previous literature, the yield is low, and the amount of solvent consumed is large, providing A new method for preparing dihydrosafrole by catalytic hydrogenation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In 1000 milliliters of reactors, add raw material safrole 15 grams, modified framework copper 10 grams, comprise phosphorus in the catalyzer, wherein with respect to the atomic ratio of copper, Cu: P is 100: 0.05, safrole And hydrogen is 45 ℃ at temperature of reaction, and with gauge pressure gauge hydrogen reaction pressure is 1.0MPa, is solvent with ethanol, solvent: safrole (weight / weight) is 6: 1, reacts 200 minutes, and its reaction result is: The conversion rate of safrole was 99.8%, and the yield of dihydrosafrole was 98.0%.

Embodiment 2～5

[0020] According to each operation step and condition of embodiment 1, just change the composition of catalyst, its reaction result is listed in table 1.

Embodiment 6

[0025] According to each step and condition of embodiment 5, just change solvent is methyl alcohol, and temperature of reaction is 60 ℃, and hydrogen reaction pressure is 0.8MPa with gauge pressure, and the reaction time is 10 hours, solvent: safrole (weight / weight) It is 4: 1, and its reaction result is: the conversion rate of safrole is 100%, and the yield of dihydrosafrole is 98.4%.

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Abstract

The catalytic hydrogenation process of preparing dihydrosafrole is one with reaction temperature of 15-100 deg.c, hydrogen pressure of 0.5-2.5 MPa, C1-C4 lower fatty alcohol and / or C6-C10 arene as solvent, and skeleton copper carrying P and at least one of B, VIB, VIII and RE elements as catalyst. The process has higher dihydrosafrole yield and less solvent consumption compared with available dihydrosafrole preparing processes and may be used in industrial production.

Description

technical field [0001] The invention relates to a method for preparing dihydrosafrole through catalytic hydrogenation, in particular to a method for preparing dihydrosafrole through hydrogenation of safrole. Background technique [0002] Dihydrosafrole has the aroma of sassafras, which can be used in tobacco, washing products and cosmetics. Its other important use is as an intermediate of methylenedioxyphenyl pesticide synergists (such as piperonyl butoxide). body. The preparation method is to carry out catalytic hydrogenation to safrole, and then carry out chloromethylation and etherification reactions. There are many kinds of catalysts used in general hydrogenation: Pd / C, Rh / C, Rh / Al 2 o 3 and Raney Ni et al. In 1931, Japan's Shozo T. et al. used reduced nickel powder to catalyze hydrogenation to obtain dihydrosafrole, but at 160-170°C and 0.6MPa, the yield was only 37%; B.B.Lurik of the former Soviet Union in 1965 Catalyzed hydrogenatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/48
Inventor 刘仲能宗弘元侯闽渤杨伟朱海燕伍艳辉
Owner CHINA PETROLEUM & CHEM CORP
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