Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4698-11-7, name is 10-Methoxy-5H-dibenzo[b,f]azepine, A new synthetic method of this compound is introduced below., Formula: C15H13NO
10-Methoxy-5H-dibenzo[b,f]azepine 4 (500 g, 2.23 mol) and isopropanol (1.0 L) were charged into a round bottomed flask and stirred for 5-10 min. 50% Aqueous hydrochloride solution (250 mL) was then added slowly to the mixture at 25-35 ?C and stirred for 15 min. The reaction mixture was heated to 60-65 ?C and maintained for 2-3 h. The progress of the reaction was monitored by TLC, and after completion of the reaction (by TLC), ethyl acetate (1.5 L) and water (1.0 L) were added into the reaction mixture and stirred for 5-10 min. Organic layer was separated and the aqueous layer was extracted with ethyl acetate (1.5 L). The combined organic layer was washed with 5% caustic lye solution (500 mL) followed by 10 % NaCl solution (500 mL) and evaporated at 50-55?C under reduced pressure. n-Hexane (500 mL) was then added into the crude product at 25-30 ?C and stirred for 1-2 h. The obtained solid was collected by filtration, washed with n-hexane (250 mL) and dried at 60-65 ?C to afford the title compound 6 as yellow solid (400 g) in 85.4% yield and >98.2% purity. Spectroscopic data were found to be in agreement with the data collected from authentic sample of intermediate 6. IR (KBR): 3329, 3284, 3040, 1643, 1474, 1309, 753 cm-1; 1H NMR (400 MHz, CDCl3): delta 3.72 (2H, s), 6.78-7.91 (8H, m); 13C NMR (400 MHz, CDCl3): delta 49.4, 119.1, 119.2, 119.8, 124.1, 124.5, 127.7, 127.9, 129.8, 130.3, 133.7, 141.5, 146.8, 190.1; HRMS calcd for C14H11NO, 210.0919; found 210.0909.
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; Ravinder; Rajeshwar Reddy; Sridhar; Murali Mohan; Srinivas, Katkam; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 22; (2013); p. 2841 – 2844;,
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