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Metal bismuth compounds, preparation method and application thereof

A technology of bismuth compounds and metals, applied in the direction of bismuth organic compounds, etc., can solve problems such as inability to form new bismuth compounds

Inactive Publication Date: 2008-09-17
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, studies have shown that Jacobsen ligands with a salen ligand structure interact with Bi 3+ Cannot form new bismuth compounds

Method used

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  • Metal bismuth compounds, preparation method and application thereof
  • Metal bismuth compounds, preparation method and application thereof
  • Metal bismuth compounds, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Compound I and its synthesis

[0025] Synthetic steps are as follows (following operations are carried out in glove box):

[0026] 1) Dissolve 0.8 mmol of the ligand compound in 2 ml of benzene and 3 ml of THF, add 0.2 mmol (0.0505 g) of NaH, and wait until no hydrogen escapes to obtain solution A;

[0027] 2) Weigh 0.805 mmol of bismuth trihalide and dissolve it in 3 ml of THF to obtain solution B;

[0028] 3) Add solution A to solution B, stir for 20-30 minutes, and react to obtain metal bismuth compound;

[0029] 4) The solvent is removed in a vacuum, and then extracted with toluene, and the product is obtained after removing the toluene from the extract, with a yield of 70%.

Embodiment 2

[0031] Compound II and its synthesis

[0032] The synthesis steps are as follows:

[0033] 1)N 2 Under protection, under ice-water bath conditions (the following additions are also carried out under ice-water bath conditions), 3.05 mmol of Na (0.0700 g) was added to 10 ml of alcohol, and the reaction was completed until hydrogen escaped;

[0034] 2)N 2 After quickly adding 1 mmol of bismuth trichloride (0.3153 grams) under protection, the solution immediately becomes a milky white suspension;

[0035] 3)N 2 Under protection, quickly add 1 mmol of ligand compound;

[0036] 4) After reacting overnight, the temperature was slowly raised to room temperature. After the reaction, the solvent was removed in a vacuum, and then extracted with toluene. The product was obtained after removing the toluene from the extract with a yield of 80%.

[0037] Metal bismuth compounds in the following examples were all prepared according to the operation steps described in Example 1 or 2.

Embodiment 3

[0039] Add 0.286 mmol Bi compound (R 1 =R 2 =t-Bu, R'=Et 2 NCH 2 CH 2 , X=Cl) and 28.6 mmoles of propylene oxide, stirred for 5 minutes and passed into CO 2 to 2.5 MPa, placed in an oil bath reactor with magnetic stirring at 120°C for reaction, after 2 hours of reaction, place the reaction kettle in a mixture of ice and water to cool the reaction liquid in the kettle. The reaction result is: the yield of propylene carbonate is 50.7%, and the selectivity of propylene carbonate is 100%.

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Abstract

The invention discloses a novel metal bismuth compound, preparation method and application thereof. The novel compound has the formula as above, i.e., contains bridge type N atom bisphenolate as the ligand, and Bi<3+> and the bridge type N atom form intramolecular coordination. The preparation method includes allowing bisphenolate [(R1)(R2)(ONa)Ph(CH2)]N[R'][(R1)(R2)(ONa)Ph(CH2)] and bismuth trihalogen to directly react if X is halogen atom to obtain objective product (I); and allowing sodium alkoxide (RCH2ONa) and bismuth trihalogen to react to produce Bi(OCH2R)3, and reacting with precursor [(R1)(R2) (OH)Ph(CH2)]N[R'][(R1)(R2)(OH)Ph(CH2)] to obtain objective product (II) if X in the formula is alkoxyl; or allowing the objective product (I) and RCH2ONa to react to produce objective product (II). The metal bismuth compound has novel structure, simple process, and high catalytic activity and selectivity for cyclic carbonate made by coupling of CO2 and epoxy compound, and has wide prospect in the fields of catalysis, organic synthesis and medicine.

Description

technical field [0001] The invention belongs to novel metallic bismuth compounds and their synthesis and application, in particular to a class of novel bismuth bisphenolate compounds and their preparation methods and applications. Background technique [0002] Bismuth (Bi) is the only heavy metal that is relatively cheap, low in toxicity and low in radioactivity. Bismuth and its compounds have some practical applications in the fields of medicine, cosmetics, catalysis, ceramics, superconducting materials, etc., and one of its main uses is as a medicament for treating digestive tract diseases. How to develop new bismuth compounds and develop new applications has become a topic of concern to chemists. [0003] Bismuth belongs to group 15 elements (formerly known as the fifth main group element), and the peripheral electronic structure is 4f 14 5d 10 6s 2 6p 3 , the main valences are +3 and +5, among which trivalent compounds are relatively stable substances in nature. Co...

Claims

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Application Information

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IPC IPC(8): C07F9/94
Inventor 尹双凤代威力罗胜联伍水生张晓文李文生
Owner HUNAN UNIV
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