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. 148017-28-1, name is tert-Butyl sulfamoylcarbamate, A new synthetic method of this compound is introduced below., 148017-28-1
Example 16 N-(4-{4-[3-(2-sulfamoylaminoethoxy)azetidin-1-yl]phenylamino}-6-methoxypyridin-3-yl)acetamide (16a) N-(4-{4-[3-(2-tert-butoxycarbonylsulfamoylaminoethoxy)azetidin-1-yl]phenylamino}-6-methoxypyridin-3-yl)acetamide N-(4-{4-[3-(2-Hydroxyethoxy)azetidin-1-yl]phenylamino}-6-methoxypyridin-3-yl)acetamide (850 mg, 2.28 mmol) produced in Example 1 (1f), N-tert-butoxycarbonylsulfamoyl amine (0.67 g, 3.4 mmol), and triphenylphosphine (0.72 g, 2.7 mmol) were suspended in ethyl acetate:tetrahydrofuran (3:1, 15 mL), diethyl azodicarboxylate (0.74 mL, 3.4 mmol) was added, and the mixture was stirred at room temperature for 20 hr. The solvent of the reaction mixture was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (chloroform:methanol, 100:0?100:4, V/V). The solvent of the object fraction was evaporated under reduced pressure to give the title object compound as a pale-yellow foam-like powder (1.05 g, yield 84%). 1H-NMR (CDCl3, 400 MHz) delta: 1.55 (9H, s), 1.96 (1H, s), 2.24 (2H, s), 3.61 (2H, t, J=5.3 Hz), 3.66-3.74 (2H, m), 3.82 (2H, s), 3.85 (1H, s), 3.98 (2H, t, J=5.3 Hz), 4.00-4.08 (2H, m), 4.38-4.46 (1H, m), 5.44-5.55 (2H, br), 6.10 (0.35H, s), 6.12 (0.35H, s), 6.15 (0.65H, s), 6.34 (0.65H, s), 6.41-6.50 (2H, m), 6.54 (0.65H, s), 6.98-7.07 (2.35H, m), 7.78 (0.65H, s), 7.79 (0.35H, s).
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:
Patent; Kyoto Pharmaceutical Industries, Ltd.; SHIRAHASE, Hiroaki; TAKAHASHI, Kenji; SHOJI, Yoshimichi; TAKEDA, Shigemitsu; (111 pag.)US2016/207883; (2016); A1;,
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