Reference of 1579-40-4, A common heterocyclic compound, 1579-40-4, name is Di-p-tolyl Ether, molecular formula is C14H14O, 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.
General procedure: To the 250 mL 3-neck RB flask charged di-p-tolylether (10 g, 50.43 mmol), benzoicacid (7.39 g, 60.52 mmol) and ZnCl2 (19.73 g, 144.73 mmol) in POCl3 (15 mL)and stirred mechanically for few minutes. Then the reaction mixture heated up to95C and allowed to stir for 4h. After 4h, color of the reaction mixture turned intodark brown and unable to stir. Then the above reaction mixture cooled to 0C andquenched with crushed ice (40 g) while mechanically stirring. To the above reactionmixture added H2O (150 ml) and allowed to stir at RT for 16h.The obtainedsolid suspension filtered through Buchner funnel and the solid cake washed withH2O (3 × 50 mL) followed by hexane (2 × 100 mL) to get crude DMPx-OH. Thiscrude solid re-dissolved in EtOAc (200 mL) and taken into separating flask andwashed with sat NaHCO3 (2 × 50 mL), the organic layer dried over Na2SO4 andevaporated the solvent on rotary evaporator to get off-white color DMPx-OH 2(10.37 g, 68%).1H NMR (400 MHz, CDCl3) delta: 2.24 (s, 6H), 2.55 (s, 1H), 7.07 (m, 4H), 7.12 (t, J= 0.8 Hz, 2H), 7.19 (m, 1H), 7.29 (m, 2H), 7.40 (dd, J1 = 8.3, 1.1 Hz, 2H).MS: 285.6 (M +).
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.
Reference:
Article; Penjarla, Srishylam; Prasad, S. Rajendra; Reddy, Dhande Sudhakar; Banerjee, Shyamapada; Penta, Santhosh; Sanghvi, Yogesh S.; Nucleosides, nucleotides and nucleic acids; vol. 37; 4; (2018); p. 232 – 247;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem