ChemicalBook CAS DataBase List ETHANOL-D

ETHANOL-D synthesis

9synthesis methods

Product Name:ETHANOL-D
CAS Number:925-93-9
Molecular formula:C2H5DO
Molecular Weight:47.07

ETHANOL-D is a deuterated NMR solvent,it can be prepared by reacting tetraethylorthosilicate with deuterium oxide.

141-78-6 Synthesis

141-78-6
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925-93-9
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Yield:-

Reaction Conditions:

with [D]-sodium hydroxide;water-d2 at 75;Inert atmosphere;

Steps:

5-6

Add 60mL (0.608mol, purity 99%) of ethyl acetate and 60mL of NaOD solution with a concentration of 11mol/L (containing 0.66mol of NaOD, the abundance of NaOD is 99.9%) into a flat-bottomed flask with a capacity of 500mL, and then add 111g (5.54 mol, abundance 99.9%) of heavy water, filled with nitrogen, stirred and refluxed at 75°C until ethyl acetate was completely hydrolyzed, the stirring speed was 550r/min, then the reaction product was transferred to an atmospheric distillation device, and replaced with nitrogen in the device The air, and then heated to collect the distillate at 165 ° C,Obtain the alcohol-water mixture of 164.4g, then the alcohol-water mixture is heated and collected the distillate under 85 , obtains the monodeuterated ethanol of 88.8g (the deuterated rate is 68.9%, and purity is 27.8%, and heavy water content is 72.2% , yield by ethanol is 51.9%, deuterium atom utilization rate is 64.7%), and the remaining liquid of distillation is reclaimed, obtains the recovery heavy water of 69.1g.

References:

CN115572211,2023,A Location in patent:Paragraph 0056-0065

64-17-5 Synthesis