The Synthesis Process of Acetonitrile-15N from Ammonium Sulfate-15N2
- 1Shanghai Research Institute of Chemical Industry CO., LTD, Shanghai 200062, China
Abstract
To address the high preparation cost and limited publicly reported synthetic processes for acetonitrile-15N as a stable isotope-labeled reagent，the synthesis process of acetonitrile-15N was investigated. Acetonitrile-15N was synthesized using ammonium sulfate-15N2 as the starting material. Ammonia-15N was first released by alkaline decomposition and absorbed in water to prepare ammonium hydroxide-15N，which was then subjected to ammonolysis with 2,2,2-trifluoroethyl acetate to afford acetamide-15N. Finally，acetonitrile-15N was obtained by dehydration distillation in the presence of phosphorus pentoxide. Based on the molar amount of ammonium sulfate-15N2 used，the overall yield of acetonitrile-15N was 68.6%. The synthesized acetonitrile-15N product was characterized and confirmed by 13C NMR,1H NMR，gas chromatography，and mass spectrometry. The chemical purity was 99.3%，and the isotopic abundance was 99.0 atom% 15N. This method features a stable raw material supply，short synthetic route，simple operation，and mild reaction conditions. It can meet the application requirements of acetonitrile-15N as a stable isotope-labeled reagent for LC-MS quantitative analysis，nitrogen isotope tracing，and the synthesis of 15N-labeled nitrogen-containing compounds.
Related
- Synthesis of the Endogenous Non-Reducing End Heparan Sulfate Disaccharides for Newborn Screening and Diagnosis of Mucopolysaccharidosis types I and II
- Catalyst‐Free Cyanation of Arenes by Acetonitrile in a Plasma–Liquid Microreactor
- Multibatch Analysis of Process Sensitivity Across Stages in 100 g Scale Mannose Triflate Synthesis
- The Sulfate-Reducing Bacteria Hypothesis in Parkinson’s Disease: From Desulfovibrio-Derived Hydrogen Sulfide to Alpha-Synuclein Aggregation
- Response to "Interpreting Route, Dose, and Clinical Relevance in Perioperative Magnesium Sulfate After Total Knee Arthroplasty" [Response to Letter].
BibTeX
@article{renzhen2026synthesis,
title = {{The Synthesis Process of Acetonitrile-15N from Ammonium Sulfate-15N2}},
author = {Renzhen FAN and Cenqi WANG and Wen LEI},
journal = {Journal of Isotopes},
year = {2026},
month = oct,
doi = {10.7538/tws.2026.youxian.052},
url = {https://doi.org/10.7538/tws.2026.youxian.052},
note = {CC BY-NC-ND},
}
RIS
TY - JOUR
TI - The Synthesis Process of Acetonitrile-15N from Ammonium Sulfate-15N2
AU - Renzhen FAN
AU - Cenqi WANG
AU - Wen LEI
PY - 2026
DA - 2026/10/26
JO - Journal of Isotopes
DO - 10.7538/tws.2026.youxian.052
UR - https://doi.org/10.7538/tws.2026.youxian.052
AB - To address the high preparation cost and limited publicly reported synthetic processes for acetonitrile-15N as a stable isotope-labeled reagent，the synthesis process of acetonitrile-15N was investigated. Acetonitrile-15N was synthesized using ammonium sulfate-15N2 as the starting material. Ammonia-15N was first released by alkaline decomposition and absorbed in water to prepare ammonium hydroxide-15N，which was then subjected to ammonolysis with 2,2,2-trifluoroethyl acetate to afford acetamide-15N. Finally，acetonitrile-15N was obtained by dehydration distillation in the presence of phosphorus pentoxide. Based on the molar amount of ammonium sulfate-15N2 used，the overall yield of acetonitrile-15N was 68.6%. The synthesized acetonitrile-15N product was characterized and confirmed by 13C NMR,1H NMR，gas chromatography，and mass spectrometry. The chemical purity was 99.3%，and the isotopic abundance was 99.0 atom% 15N. This method features a stable raw material supply，short synthetic route，simple operation，and mild reaction conditions. It can meet the application requirements of acetonitrile-15N as a stable isotope-labeled reagent for LC-MS quantitative analysis，nitrogen isotope tracing，and the synthesis of 15N-labeled nitrogen-containing compounds.
SN - 1000-7512
ER -