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The Production Process of Bis(10-hydroxybenzo[h]quinolinato)beryllium
Bis(10-hydroxybenzo[h]quinolinato)beryllium, also known as Berlocq reagent, is a widely used ligand in coordination chemistry and metal organic frameworks (MOFs).
It is used as a ligand for the preparation of transition metal complexes, including those of ruthenium, osmium, and iridium.
The synthesis of Berlocq reagent involves a multi-step process that involves the reaction of several chemicals.
Step 1: Preparation of 10-hydroxybenzo[h]quinoline
The first step in the synthesis of Berlocq reagent involves the preparation of 10-hydroxybenzo[h]quinoline.
This compound is prepared by the hydroxylation of 1,4-benzoquinone using aqueous hydrogen peroxide in the presence of a catalyst, such as sodium hydroxide or sulfuric acid.
The reaction is carried out at room temperature and the product is isolated by filtration and washing with water.
Step 2: Hydrolysis of 10-hydroxybenzo[h]quinoline
The 10-hydroxybenzo[h]quinoline prepared in the previous step is then subjected to hydrolysis to produce the desired product, which is 10-hydroxybenzo[h]quinolinate.
This is achieved by treating the 10-hydroxybenzo[h]quinoline with a strong acid, such as hydrochloric acid, in the presence of water.
The reaction is carried out at room temperature, and the product is isolated by filtration and washing with water.
Step 3: Chlorination of 10-hydroxybenzo[h]quinolinate
In the third step, the 10-hydroxybenzo[h]quinolinate obtained in the previous step is treated with chlorine gas in the presence of a solvent, such as benzene or toluene.
The reaction is carried out at a temperature below room temperature, such as 0°C, and the product is isolated by filtration and washing with a solvent.
Step 4: reaction with Beryllium salt
The final step in the synthesis of Berlocq reagent involves the reaction of the 10-hydroxybenzo[h]quinolinate obtained in the previous step with a beryllium salt, such as beryllium nitrate or beryllium chloride.
The reaction is carried out in the presence of a catalyst, such as sodium hydroxide, and the product is isolated by filtration and washing with water.
Overall, the synthesis of Berlocq reagent involves a multi-step process that requires the use of several chemicals and reagents.
The synthesis of the starting material, 10-hydroxybenzo[h]quinoline, is the most critical step in the synthesis of Berlocq reagent.
The reaction involves the use of hydrogen peroxide, a strong acid, chlorine gas, and a beryllium salt.
The final product is isolated by filtration and washing with water.
The reaction is carried out at different temperatures and the product is isolated by filtration and washing with different solvents.
The synthesis of Berlocq reagent requires some careful handling and should be carried out in a well-ventilated area with appropriate safety precautions.
The product is then used as a ligand for the preparation of transition metal complexes, including those of ruthenium, osmium, and iridium.
In summary, Berlocq reagent is a widely used ligand in coordination chemistry and metal organic frameworks (MOFs).
The synthesis of Berlocq re