Anhydrous methylene chloride

Solvents were purchased from Sigma Aldrich, Combi blocks, Oakwood chemicals, Alfa Aesar, VWR and Thermofisher. Anhydrous methylene chloride (DCM), anhydrous tetrahydrofuran (THF) and anhydrous DMF were purchased from Sigma Aldrich. Reactions were monitored using Opt. KMnO4 glass-based Silica Plates, F254 thin layer chromatography plates (TLC) and column purification was done using silica gel chromatography (TLG-R10014BK-323) purchased from Silicycle. NMR spectra were recorded on a Bruker 400 MHz Spectrometer using CDCl3, D2O (Sigma Aldrich), as d-solvents and internal standards (δ 7.26 for 1 H NMR and δ 77.00 for 13 acrylate 46 (4) (3.13 mmol, 0.40 g), were added to an oven dried 5ml biotage microwave vial and solvent free conditions were maintained 46 . The sealed microwave vial was stirred for 2-3 days at 90°C. Reaction progress was monitored by TLC (chloroform/methanol 9:1 v/v, can be visualized with iodine stain, and Phospomolybdic Acid stain), until complete consumption of 1. The crude product was purified on a silica gel column eluted with chloroform containing 0-5% methanol.
Column fractions were analyzed by thin layer chromatography (TLC) and fractions containing pure product (Rf = 0.34) were concentrated, to obtain product as yellow oil ( 5). (0.30 g, 53% yield).