Hello ACS Community,
I hope this message finds you well. I am currently working on a project involving the synthesis of 2,4-Dinitrophenylhydrazine (DNPH), and I have encountered some challenges that I hope to get advice on.
Background:
- The goal of my project is to synthesize 2,4-Dinitrophenylhydrazine using a standard diazotization method followed by reduction.
- I have been following the protocol outlined in [reference paper/standard method], but I am experiencing lower-than-expected yields and some impurities in the final product.
Details:
- Reagents: 2,4-Dinitrochlorobenzene, hydrazine hydrate, and solvents like ethanol and water.
- Conditions: Diazotization at 0-5°C, reduction at room temperature.
- Observations: The reaction mixture turns dark red, and the final product shows unexpected byproducts on TLC.
Challenges:
- Yield: The yield is consistently lower than reported in the literature, around 50% compared to the expected 80%.
- Purity: The NMR and HPLC analyses show the presence of impurities, which I believe might be unreacted starting materials or side products.
Questions:
- Has anyone experienced similar issues with this synthesis method, and how did you overcome them?
- Are there any modifications to the protocol that you would recommend to improve yield and purity?
- Could the impurities be a result of incomplete reduction or side reactions, and how can I test for this?
Any insights, suggestions, or references to relevant literature would be greatly appreciated. I am eager to learn from the community's expertise and improve my synthesis process.
Thank you in advance for your help!
