FLUCONAZOLE IMPURITY C synthesis
- Product Name:FLUCONAZOLE IMPURITY C
- CAS Number:514222-44-7
- Molecular formula:C10H8N6
- Molecular Weight:212.21
288-36-8
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$6.00/1g
108-36-1
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$10.00/1g
514222-44-7
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$125.00/5mg
Yield: 79%
Reaction Conditions:
with copper(l) iodide;N,N-dimethyl-ethanamine;potassium carbonate in dimethyl sulfoxide at 150; for 36 h;Inert atmosphere;
Steps:
2.2 Synthesis of ligand 1,3-bis(1,2,4-triazol-1-yl)benzene (btb)
1,3-Dibromobenzene (0.75g, 3.2mmol), triazole (2.18g, 12.8mmol), K2CO3 (2.96g, 21.0mmol), CuI (0.03g, 0.13mmol) and 7 drops of N,N’-dimethyl ethane amine were mixed in 15ml dry DMSO solution and heated at 150°C for 36h under a nitrogen atmosphere. The mixture was cooled to room temperature, filtered and the solid was washed with DMSO. The filtrate was distilled under reduced pressure to remove the solvent and the residue was extracted with CH2Cl2 (6×30mL). The organic layer was separated, dried over magnesium sulfate, and evaporated to dryness to give the crude product, which was further separated under column chromatography to give 0.54g of btb. Yield: 79%; 1H NMR [CDCl3]: 8.61 (s, 2H), 8.09 (s, 2H), 7.67 (dd, 2H), 7.62 (s, 1H); 7.59 (t, 1H) ppm; elemental analysis calcd (%) for C10H8N6: C 56.59, H 3.80, N 39.61; found C 56.37, H 3.68, N 39.42.
References:
Shi, Xiu Juan;Chen, Peng Yun;Yin, Zhen Ming;Li, Tuo;Wu, Ming Ze;Tian, Li [Polyhedron,2018,vol. 141,p. 87 - 93]
288-88-0
781 suppliers
$10.00/5g
108-36-1
445 suppliers
$10.00/1g
514222-44-7
81 suppliers
$125.00/5mg