Ethyl Ester Synthesis Lab Report

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Ethyl vinyl ether was used to protect –OH on glycidol based on a literature reported protocal.59 In a typical procedure, 0.675 mol glycidol and 200 mL ethyl vinyl ether were loaded in a round-bottom flask, to which 1.25 g TsOH was then added. The reaction was allowed to proceed at room temperature (RT) for 3h. The resulting mixture was then purified by washing with 100 ml saturated aqueous solution of NaHCO3 for 3 times. The organic layer obtained was dried by MgSO4. After filtration of MgSO4, the excess ethyl vinyl ether was removed by rotary evaporation. The fraction at 51 °C /80 Pa from the remaining solution was collected under reduced pressure distillation. The final product EEGE monomer is a colorless liquid (Yield: 76 %).

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In a typical example, 1 g c-PEO-OH was dissolved in 30 mL anhydrous N-Methyl-2-pyrrolidone (NMP) solvent under dry argon atmosphere, to which 10 mL 2-bromoisobutyryl bromide was added at 0 °C dropwise for 30 min under vigorous stirring. The reaction mixture was then allowed to proceed at room temperature for 1 d. After that, the solution was concentrated by reduced pressure distillation to remove NMP solvent and excess 2-bromoisobutyryl bromide. The crude product was then washed with saturated aqueous solution of NaHCO3 and water sequentially for 3 times, dried over MgSO4, and precipitated in cold n-hexane to obtain a final brown viscous product.

Preparation of c-PEO-N3 by substituting the Br on c-PEO-Br with azide functionalities
Typically, c-PEO-Br (0.55g) and NaN3 (0.73g) were dissolved in 20 ml DMF in a flask. The mixture was reacted at room temperature for 24 h. After the reaction is complete, the mixture was filtered through a column of neutral alumina with dichloromethane as eluent. The solution was then concentrated under reduced pressure to remove the solvents, and finally precipitated in cold n-hexane for three times to obtain the purified product c-PEO-N3.

Synthesis of ethynyl-terminated poly(3-hexylthiophene) (P3HT) by Grignard Metathesis method

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