4-Imidazolemethanol hydrochloride synthesis
- Product Name:4-Imidazolemethanol hydrochloride
- CAS Number:32673-41-9
- Molecular formula:C4H7ClN2O
- Molecular Weight:134.56
50-00-0
96-26-4
32673-41-9
A solvent mixture of acetonitrile and ethanol with a volume ratio of 2:1 was added to the reactor, and 100 mmol of 1,3-dihydroxyacetone and 200 mmol of formaldehyde were added sequentially and stirred until complete dissolution. Subsequently, 100 mmol of ceric ammonium nitrate was added as an oxidizing agent. The pH of the reaction system was adjusted to 10 by slow dropwise addition of sodium ethanolate solution at atmospheric pressure and 60 °C, and 15 mmol of catalyst was added. The reaction was stirred under this condition for 8 hours, and 4-hydroxymethylimidazole was obtained after completion of the reaction. To the reaction solution, concentrated hydrochloric acid was added dropwise to adjust the pH to 2, and the precipitate was collected by filtration. The solid was washed with saturated sodium chloride solution and subsequently recrystallized with ethanol. Finally, the product was dried under vacuum to obtain 4-hydroxymethylimidazole hydrochloride. The purity of the product was determined to be 98.2% and the yield was 87.5%.
Yield:32673-41-9 87.5%
Reaction Conditions:
with hydrogenchloride;ammonium cerium (IV) nitrate;sodium ethanolate in ethanol;acetonitrile; pH=10 at 60; for 8 h;Reagent/catalyst;
Steps:
3 Example 3
A mixture of acetonitrile and ethanol in a volume ratio of 2: 1 was added to the reactor,100 mmol of 1,3-dihydroxyacetone and 200 mmol of formaldehyde were dissolved in an organic solvent,100 mmol of cerium ammonium nitrate was added,Under normal pressure 60 conditions,Adding sodium ethoxide to adjust the pH to 10,15 mmol of catalyst was added,Stirring reaction 8h, obtained 4-hydroxymethyl imidazole,After completion of the reaction,Dropping concentrated HCl,Adjust pH = 2,filter,The filtered solid,Washed with saturated brine,Recrystallization from ethanol,Dried in vacuo to give the product 4-hydroxymethylimidazole hydrochloride.The purity of the prepared 4-hydroxymethylimidazolidine hydrochloride was 98.2%The yield was 87.5%.
References:
Ye, Fang CN106349165, 2017, A Location in patent:Paragraph 0016-0030
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