Electric Literature of 102-52-3, A common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
To a suspension of intermediate lId (1.834 g, 8.94 mmol) in EtOH (30 ml) were added malonaldehyde bis(dimethyl acetal) (1.63 ml, 9.84 mmol) and conc.HC1 (1 ml). The reaction mixture was stilTed at 70C for 2 hours. The cooled mixture was evaporated todryness, diluted saturated solution of NaHCO3 and extracted with EtOAc twice. The combined organics were washed with water, with saturated solution of NaC1, dried over MgSO4, filtered and evaporated. The final product was purified by silica gel chromatography using 0 to 30 % EtOAc/cyclohexane as eluent to give intermediate lie(1.380 g, 64%). ?H NMR (500 MHz, CDC13) oe 8.12 (d, J= 2.1 Hz, 1H), 7.94 (s, 1H), 7.85 (d, J= 8.3 Hz, 1H), 7.72 (d, J= 1.4 Hz, 1H), 7.40 (s, 1H), 7.36 (dd, J= 8.3, 1.8 Hz, 1H),7.32 (d, J= 1.7 Hz, 1H), 6.46-6.43 (m, 1H), 3.97 (s, 3H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.