Ethyl 5-Methyl-1,3,4-thiadiazole-2-carboxylate synthesis
- Product Name:Ethyl 5-Methyl-1,3,4-thiadiazole-2-carboxylate
- CAS Number:869108-50-9
- Molecular formula:C6H8N2O2S
- Molecular Weight:172.2
42042-84-2
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869108-50-9
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Yield: 28%
Reaction Conditions:
with Lawessons reagent in tetrahydrofuran at 75; for 3 h;
Steps:
Preparation of ethyl 5-methyl-1 ,3,4-thiadiazole-2-carboxylate.
To a solution of ethyl 2-(2-acetylhydrazinyl)-2-oxoacetate (3 g, 17 mmol) in THF (100 mL) was added Lawesson's reagent (7.66 g, 19 mmol) . The mixture was stirred at 75°C for 3 hours. The mixture was diluted with ethyl acetate (500 mL) and added approximately 40 g of decolourising charcoal. The mixture was stirred at 18°C for 16 hours. The mixture was filtered. The filtrate was concentrated under vacuo. The residue was purified with column chromatography (Si02, petroleum ether:ethyl acetate = 3:7) to give ethyl 5-methyl-1 ,3,4- thiadiazole-2-carboxylate (921 mg, 28% yield).
References:
H. LUNDBECK A/S;KEHLER, Jan;JUHL, Karsten;MARIGO, Mauro;VITAL, Paulo, Jorge, Vieira;JESSING, Mikkel;LANGGÅRD, Morten;RASMUSSEN, Lars, Kyhn;CLEMENTSON, Carl, Martin, Sebastian WO2018/7249, 2018, A1 Location in patent:Page/Page column 94
1068-57-1
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4755-77-5
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869108-50-9
61 suppliers
$45.00/25mg