ChemicalBook CAS DataBase List Benzene-D6

Benzene-D6 synthesis

12synthesis methods

Product Name:Benzene-D6
CAS Number:1076-43-3
Molecular formula:C6D6
Molecular Weight:84.15

BENZENE-D6 is synthesized by the following steps：The hexahalogenated benzene was prepared to obtain a clear solution and transferred to an autoclave. The deuterated reagent B was slowly added to the solution, and then the 78.8 ℃ fraction was obtained the benzene d6.

392-56-3 Synthesis

392-56-3
296 suppliers
$9.00/1g

1076-43-3
227 suppliers
$21.00/10x0.5ml

Yield:1076-43-3 88.9%

Reaction Conditions:

with lithium aluminium deuteride;palladium on activated charcoal;deuterium in tetrahydrofuran at 25 - 70; under 15001.5 Torr; for 24 h;Autoclave;

Steps:

5 Example 5

In a dry room temperature environment, 27.9g of hexafluorobenzene was slowly added to 2500g of anhydrous tetrahydrofuran, stirred at 250rpm, after stirring for 1 hour, a clear solution A was obtained; the clear solution A was transferred to a 6L autoclave Under the protection of nitrogen, slowly add 75.6 g of lithium aluminum deuteride to the clear solution A. During the addition, keep the solution temperature not higher than 25. After the addition of lithium aluminum deuteride is completed, add 2.8 to the mixed solution. gPlatinum-carbon catalyst, after no bubbles emerge in the solution, seal the reaction system and check the air-tightness of the device. Then replace the gas in the autoclave with deuterium gas. After replacement 3 times, fill the autoclave with deuterium gas. When the pressure reaches 2MPa, close the inlet valve, stir at 500rpm and increase the temperature to 70. After keeping for 24 hours, stop stirring and cool to room temperature naturally; filter and transfer the filtrate to a 6L three-port pressure device And place it in a high precision medium temperature circulating bath of -5, slowly drip 5 deionized water into the filtrate through a constant pressure dropping funnel at a rate of 5mL/min. When no bubbles are generated, stop the dripping and add to the solution Three zeolites were added to fractionate the solution, and the solution was heated at a heating rate of 5°C/min. A fraction of 78.8°C was taken to obtain 9.0 g of benzene-d6. The product yield was 88.9% and the purity was 99.5%.

References:

CN111592442,2020,A Location in patent:Paragraph 0028; 0029

87-82-1 Synthesis