Ethyl Ester Synthesis Lab Report
Synthesis …show more content…
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