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ChemicalBook CAS DataBase List N-(4-BroMo-phenyl)-benzene-1,2-diaMine
100953-52-4

N-(4-BroMo-phenyl)-benzene-1,2-diaMine synthesis

7synthesis methods
-

Yield: 100%

Reaction Conditions:

with sodium hydrogensulfite in tetrahydrofuran;methanol;water at 20;Inert atmosphere;

Steps:

6.2
(6-2) Synthesis of Intermediate A6; To a solution of 15 g (51 mmol) of Intermediate A5 in 150 mL of tetrahydrofuran, a solution of 45 g (0.26 mol) sodium hydrosulfite in 150 mL of water was added dropwise in argon atmosphere at room temperature under stirring and 10 mL of methanol was further added to continue the stirring for 3 h. After the reaction solution turned transparent to show the completion of the reaction, 200 mL of ethyl acetate was added and the solution was neutralized by a sodium hydrogencarbonate aqueous solution. The organic layer separated was washed with a saturated saline solution and dried over anhydrous magnesium sulfate, and then, the solvent was evaporated off under reduced pressure to obtain 13.5 g of Intermediate A6. Yield: 100%.

References:

Idemitsu Kosan Co., Ltd. EP2236501, 2010, A1 Location in patent:Page/Page column 38