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ChemicalBook CAS DataBase List 4-(N-ETHYLSULPHONAMIDO)BENZENEBORONIC ACID
871329-65-6

4-(N-ETHYLSULPHONAMIDO)BENZENEBORONIC ACID synthesis

2synthesis methods
-

Yield:871329-65-6 40%

Reaction Conditions:

with n-butyllithium in tetrahydrofuran at -70 - 0;

Steps:

51i.2 Step 2: [4-(ethylsulfamoyl)phenyl]boronic acid (3)

To a solution of 4-bromo-N-ethylbenzenesulfonamide (2, 1.06 g, 4.01 mmol) and triisopropyl borate (1.39 mL, 6.02 mmol) in tetrahydrofuran (20.1 mL) was added n-Butyl Lithium (4.01 mL, 10.0 mmol) at -70° C. The mixture was slowly warmed to 0° C, then 10% HCl solution was added until pH 3-4. The resulting mixture was extracted with EtOAc and the extract washed with brine, dried over Na2SO4, filtered and the solvent removed under reduced pressure. The residue was triturated with diethyl ether to yield [4- (ethylsulfamoyl)phenyl]boronic acid (368 mg, 1,61 mmol, 40% yield). (0796) Analytical data: 1H NMR (200 MHz, DMSO) δ 8.41 (s, 2H), 7.94 (d, J = 8.1 Hz, 2H), 7.74 (d, J = 8.1 Hz, 2H), 7.52 (t, J = 5.7 Hz, 1H), 2.87- 2.67 (m, 2H), 0.93 (t, J = 7.2 Hz, 3H); (0797) 13C NMR (50 MHz, DMSO) δ 142.1, 135.0, 125.7, 37.9, 15.0.

References:

WO2019/149738,2019,A1 Location in patent:Page/Page column 75; 76

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