3-Methylpyrazole synthesis

8synthesis methods

Product Name:3-Methylpyrazole
CAS Number:1453-58-3
Molecular formula:C4H6N2
Molecular Weight:82.1

13808-64-5
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$6.00/1g

1453-58-3
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$6.00/5g

Yield:1453-58-3 > 95 %Chromat.

Reaction Conditions:

with methanol;sodium tetrahydroborate;Pd/AlO(OH);water at 20; for 2 h;Sonication;Schlenk technique;

Steps:

4.3. General procedure for the dehalogenation reactions

First, Pd/AlO(OH) NP catalyst (40.0 mg, 0.16 mmol %) and 1 mL of H₂O/MeOH (v/v = 1/1) were added to a Schlenk tube. Next, the halogenated compound (0.25 mmol) was added. Finally, NaBH₄ (0.75 mmol) was added to the reaction mixture and the vessel was closed. The reaction then continued during vigorous stirring under ultrasonic conditions at room temperature and was monitored by GC. Most of the reactions were completed over a time period of 1.5 - 4 h. After completion of the reaction, the catalyst was removed via simple centrifugation at 6000 rpm and then washed three times with methanol and water and allowed to dry for further use. The solvent was evaporated under vacuum. The products were purified by flash column chromatography and the dehalogenated products were then determined by ¹H NMR.

References:

Kara, Belguzar Yasemin;Yazici, Melike;Kilbas, Benan;Goksu, Haydar [Tetrahedron,2016,vol. 72,# 39,p. 5898 - 5902]

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