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17th April 2019 @ 10:15

2-chloro-3-(4-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyrazine was synthesised from the previously synthesised 2-chloro-6-(2-hydrazinyl)(4-chlorobenzylidene)pyrazine intermediate.

Reaction Scheme

Reaction 2 scheme.png

Risk assessment

4chlorobenzaldehyde reaction 2 risk assessment.pdf

Reagents

                                                                                     mass/g      moles/mmol       equivalents

2-chloro-6-(2-hydrazinyl)(4-chlorobenzylidene)pyrazine       0.0201       0.062                   1.0

diacetoxyiodobenzene                                                            0.0310       0.096                   1.5

Proceedure

A round bottomed flask was charged with Synthesis of 2-Chloro-6-(2-hydrazinyl)(4-chlorobenzylidene)pyrazine (0.0212 g, 0.067 mmol), diacetoxyiodobenzene (0.0250 g, 0.078 mmol) and dichloromethane (10 mL) in. The resulting solution was stirred at room temperature and monitored using TLC (7: 3 ethyl acetate: light petroleum ether solvent used) until completion. The resulting product was then isolated by column chromatography, using the same solvents (Rf = 0.4) and dried via vacuum filtration yielding a white powder (0.0181g, 85.7%). The product was characterised via 1H and 13C NMR, infrared and melting point analysis.

Analytical Data

4chlorobenzaldehyde reaction2 H NMR spectrum.pdf

4chlorobenzaldehyde reaction2 IR spectrum.pdf

4chlorobenzaldehyde reaction2 Mass spectrum.pdf

4chlorobenzaldehyde reaction2 C NMR spectrum.pdf

Mpt = 261-265C

Inchi keys

2-chloro-6-(2-hydrazinyl)(4-chlorobenzylidene)pyrazine IREXIIXDQDGVMX-UHFFFAOYSA-N

diacetoxyiodobenzene  ZBIKORITPGTTGI-UHFFFAOYSA-N

2-chloro-3-(4-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyrazine VCWFDFYRPOTNNX-UHFFFAOYSA-N

Attached Files
4chlorobenzaldehyde reaction 2 risk assessment.pdf
4chlorobenzaldehyde reaction2 H NMR spectrum.pdf
4chlorobenzaldehyde reaction2 IR spectrum.pdf
4chlorobenzaldehyde reaction2 Mass spectrum.pdf
4chlorobenzaldehyde reaction2 C NMR spectrum.pdf
Reaction 2 scheme.png