2.3. Synthesis of 2,3,4,5-Tetrabromothiophene (Th-Br4)

MM Mohamed Gamal Mohamed
HH Huan-Yu Hu
MM Manivannan Madhu
ME Mohsin Ejaz
SS Santosh U. Sharma
WT Wei-Lung Tseng
MS Maha Mohamed Samy
CH Cheng-Wei Huang
JL Jyh-Tsung Lee
SK Shiao-Wei Kuo
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Br2 (5.3 mL, 0.033 mmol) and Th (2.0 g, 0.023 mmol) were dissolved in CHCl3 (30 mL) and then the mixture was refluxed for 24 hours at 0 ℃. After cooling, the solution mixture was added to cool, saturated sodium thiosulfate. The obtained solid was purified in hot ethanol to remove any impurities from the monomer to obtain Th-Br4 as a white powder (Figure 1, 80%, Tm: 119 °C). FTIR (KBr, cm–1, Figure 2a): 1636 (C=C), 852 (C–S). 1H NMR (500 MHz, DMSO, δ, ppm, Figure S2): No peak was detected. 13C NMR (125 MHz, CDCl3, δ, ppm, Figure 2b): 116.936, 110.284.

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