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Preparation of tri(alkoxyphenyl)bismuth compounds

A technology of alkoxyphenyl and alkoxybromobenzene, which is applied in the field of preparation of tri-bismuth series compounds to achieve the effects of reducing pollution, saving costs, and good safety

Inactive Publication Date: 2009-04-22
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This invention relates to improving methods for producing high purity metallic tin by reacting titania with hydrogen fluoride gas under specific conditions. By mixing these two liquids together beforehand, there will be fewer steps needed during manufacturing processes while still achieving desired results. Additionally, this method allows for more efficient activation of metal particles when compared to other techniques such as adding ethers.

Problems solved by technology

Technological Problem addressed by this patents relating to the current process of producing small solid rocket motors involves complex processes involving multiple steps like synthesis, grinding, and final assembly into products. These factors contribute to increased costs associated with these manufacturing techniques. Additionally, there may also result from unstable chemicals during storage and handling, leading to decomposition and reduced reliability over time.

Method used

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  • Preparation of tri(alkoxyphenyl)bismuth compounds
  • Preparation of tri(alkoxyphenyl)bismuth compounds

Examples

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Embodiment 1

[0019] The preparation of embodiment 1. three-(p-ethoxyphenyl) bismuth

[0020] In a 1L dry reaction flask, add 29.3 grams (1.205mole) of magnesium chips and 80ml of THF (cover the magnesium chips), add 242.3 grams (1.205 mole) of p-EtO-C in the high dropping funnel 6 h 4 A mixed solution of Br and 230ml THF was added dropwise with slow stirring under nitrogen protection, while heating carefully to initiate the reaction. After the reaction occurs, control the rate of addition to keep the reaction in a slightly boiling state. The reaction temperature can reach 90 ° C ~ 120 ° C. After about 1 hour, the dropwise addition is completed and the reaction is continued for about 2.5 hours at the temperature of an oil bath at 120 ° C to fully generate p-EtOC 6 h 4 MgBr Grignard reagent. Then, 123 grams (0.39 mole) of anhydrous BiCl in the high-position dropping funnel was mixed under stirring condition 3 The emulsified solution prepared with 240ml THF was added dropwise to the Grign...

Embodiment 2

[0021] Embodiment 2. the preparation of three-(ortho-ethoxyphenyl) bismuth

[0022] In a 1L dry reaction flask, add 13.5g (0.556mole) magnesium chips and 60ml THF (cover the magnesium chips), add 111.8g (0.556mole) o-EtO-C 6 h 4 A mixed solution of Br and 150ml THF was added dropwise under nitrogen protection with slow stirring and carefully heated to initiate the reaction. After the reaction occurs, control the dripping speed to keep the reaction in a slightly boiling state. The reaction temperature can reach 90 ° C ~ 120 ° C. It takes about 0.5 hours to complete the dropwise addition and continue to react for about 1.5 hours at 120 ° C oil bath temperature to fully generate o- EtOC 6 h 4 MgBr Grignard reagent. Then 57g (0.181mole) of anhydrous BiCl in the high position dropping funnel was mixed under stirring condition 3 The emulsified solution prepared with 150ml THF was added dropwise to the Grignard reagent for metal transfer reaction, and the addition was completed ...

Embodiment 3

[0023] Embodiment 3. the preparation of three-(m-ethoxyphenyl) bismuth

[0024] In a 1L dry reaction flask, add 25.2g (1.0356mole) magnesium chips and 80ml THF (cover the magnesium chips), add 208.1g (1.035mole) m-EtO-C 6 h 4 A mixed solution of Br and 200ml THF was added dropwise under nitrogen protection with slow stirring and carefully heated to initiate the reaction. After the reaction occurs, control the rate of addition to keep the reaction in a slightly boiling state. The reaction temperature can reach 90°C to 120°C. The dropwise addition is completed in about 1 hour, and the reaction is kept at 120°C for about 2.5 hours in an oil bath to fully generate m-EtO- C 6 h 4 MgBr Grignard reagent. Then 105.6g (0.335mole) of anhydrous BiCl in the high position dropping funnel was mixed under stirring condition 3 Add the emulsified solution prepared with 210ml THF dropwise into the Grignard reagent for the metal transfer reaction, finish the addition in about 1 hour and kee...

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Abstract

The invention relates to a method for preparing a 3-(alkoxy phenyl) bismuth serial compound. An alkoxy brombenzene serial compound is used as a raw material; under the protection of nitrogen gas, the alkoxy brombenzene serial compound in an anhydrous solvent and magnesium chips are subjected to Grignard reaction to generate an alkoxy phenyl magnesium bromide Grignard reagent; and the alkoxy phenyl magnesium bromide Grignard reagent and anhydrous bismuth trichloride undergo metal transferring reaction to prepare the 3-(alkoxy phenyl) bismuth serial compound. The alkoxy brombenzene serial compound comprises p-BrC6H4OMe, o-BrC6H4OMe, p-BrC6H4OEt, o-BrC6H4OEt or m-BrC6H4OEt. An organic solvent with high boiling point is safer than aether and can activate the magnesium chips; in particular, THF is adopted to emulsify and dissolve anhydrous BiCl3 and is favorable for preparation operation; the reclaimed THF can be used for subsequent extraction, save raw materials and reduce pollution; and the method has mild reaction condition and uncomplicated technical requirement, and is favorable for industrialized preparation.

Description

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Claims

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Application Information

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Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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