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Method for synthesizing 1,2-dimethoxy-1-phenylethane

A synthesis method and technology of phenylethane, applied in the field of organic compound synthesis, can solve the problems of long reaction time, complicated reaction process, expensive catalyst and the like, and achieve the effects of simple operation, broad application prospect and feasible process

Active Publication Date: 2014-08-13
杭州坚膜新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the disadvantages of complex reaction process, long reaction time and expensive catalyst mentioned in the above documents, and provide a 1,2-bis The synthetic method of methoxy-1-phenylethane

Method used

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  • Method for synthesizing 1,2-dimethoxy-1-phenylethane
  • Method for synthesizing 1,2-dimethoxy-1-phenylethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Preparation of solid acid catalyst:

[0024] Weigh 12.8g of ZrOCI 2 ·8H 2 O in a beaker, add a certain amount of water and ethanol (volume ratio 3:1) to make a solution with a mass fraction of 8%, after mixing evenly, add concentrated ammonia water dropwise to the solution under rapid stirring, and adjust the pH to 9 , the solution was formed into a gel, and the gel was aged at room temperature for 24 hours, filtered with suction, and washed repeatedly until no Cl - . Put the precipitate in an oven and dry at 120°C for 10-12 hours to obtain a solid powder, then grind the powder, impregnate it with 0.5mol / L sulfuric acid solution (15ml / g catalyst) for 12 hours, and filter Then dry it, and bake it in a muffle furnace at 530°C for 3 hours to obtain SO 4 2- / ZrO 2 type solid acid catalyst.

[0025] 2. Catalytic reaction

[0026] Put 1 gram of the catalyst prepared in (1) into the reaction vessel, add 23 milliliters (0.2mol) of m-xylene, 80.9 milliliters (2mol) of...

Embodiment 2

[0028] 1. Preparation of solid acid catalyst:

[0029] Weigh 12.8g of ZrOCI 2 ·8H 2 O and 8.0g of Fe(NO 3 ) 3 9H 2 O in a beaker, add a certain amount of water and ethanol (volume ratio 3:1) to make a solution with a mass fraction of 8%, after mixing evenly, add concentrated ammonia water dropwise to the solution under rapid stirring, and adjust the pH to 9 , the solution was formed into a gel, and the gel was aged at room temperature for 24 hours, filtered with suction, and washed repeatedly until no Cl - . Put the precipitate in an oven and dry at 130°C for 10-12 hours to obtain a solid powder, then grind the powder, impregnate it with 0.5mol / L sulfuric acid solution (15ml / g catalyst) for 12 hours, and filter Then dry it, and bake it in a muffle furnace at 510°C for 3 hours to obtain SO 4 2- / ZrO 2 -Fe 2 o 3 type solid acid catalyst.

[0030] 2. Catalytic reaction

[0031] Put 1 gram of the catalyst prepared in (1) into the reaction vessel, add 23 milliliters (...

Embodiment 3

[0033] 1. Preparation of solid acid catalyst:

[0034] Weigh 12.8g of ZrOCI 2 ·8H 2 O and 12ml of C 16 h 36 o 4 Put Ti in a beaker, add a certain amount of water and ethanol (volume ratio 3:1) to make a solution with a mass fraction of 8%, after mixing evenly, add concentrated ammonia water dropwise to the solution under rapid stirring, and adjust the pH=9 , the solution was formed into a gel, and the gel was aged at room temperature for 24 hours, filtered with suction, and washed repeatedly until no Cl - . Put the precipitate in an oven and dry at 110°C for 10-12 hours to obtain a solid powder, then grind the powder, impregnate it with 0.5mol / L sulfuric acid solution (with 15ml / g catalyst) for 12 hours, and filter Then dry it, and bake it in a muffle furnace at 510°C for 3 hours to obtain SO 4 2- / ZrO 2 -TiO 2 type solid acid catalyst.

[0035] 2. Catalytic reaction

[0036] Put 1 gram of the catalyst prepared in (1) into the reaction vessel, add 23 ml (0.2 mol) m-x...

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Abstract

The invention discloses a method for synthesizing chemical substances, in particular to a method for synthesizing 1,2-dimethoxy-1-phenylethane by applying electrochemical catalytic oxidation technology. In the present invention, ZrOCl2·8H2O is used as raw material to prepare SO42- / ZrO2 type solid acid catalyst, and then the catalyst is added to the reaction material composed of styrene and methanol, wherein the molar ratio of styrene and methanol is 1:10; When the flat graphite is used as the electrode and the electricity is applied, the reaction is carried out to lift the product, and then the subsequent steps of separation and the like can be carried out. The invention has the advantages of reasonable process design, feasible process, simple and convenient operation, mild reaction conditions, and a high-yield and high-selectivity product can be synthesized by a one-pot cooking method at normal temperature and pressure. The invention can be widely used in chemical enterprises.

Description

technical field [0001] The invention relates to a method for synthesizing chemical substances, in particular to the synthesis of organic compounds using electrochemical catalytic oxidation technology. technical background [0002] 1,2-Dimethoxy-1-phenylethane has many uses as a fine chemical product, not only widely used as flavor in cosmetics or food, but also as a good gasoline additive. The current main report on the synthesis of 1,2-dimethoxy-1-phenylethane: Kambe Nobuaki reported some 1,2 in Chemistry Letters in 1987 and Phosphorus and Sulfur and the Related Elements in 1988 -The synthesis method of dimethoxy-1-phenylethane, but their reaction time is long, the reaction process is complicated, and expensive diphenyl ditellurium is used as a catalyst, and concentrated sulfuric acid and tert-butyl peroxide are used Reagent, not green, low-carbon and energy-saving. [0003] [0004] From the perspective of seeking the widest application of methanol and solving future ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/02C25B3/23
Inventor 陈锋涛张云飞
Owner 杭州坚膜新材料有限公司