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ChemicalBook CAS DataBase List (5-BROMO-3-NITRO-PYRIDIN-2-YL)-METHYL-AMINE
70232-59-6

(5-BROMO-3-NITRO-PYRIDIN-2-YL)-METHYL-AMINE synthesis

8synthesis methods
-

Yield:70232-59-6 100%

Reaction Conditions:

in tetrahydrofuran at 0; for 0.5 h;

Steps:

63.1

63a (3 g, 1.0 eq) is dissolved in THF (13 mL), and then cooled to 0° C. Methylamine solution (2M in THF, 20.8 mL, 3.3 eq), is slowly added to the reaction mixture (exothermic). The reaction mixture is stirred for 30 min at 0° C. and diluted with EtOAc. Organic layer is washed with sat aq sodium bicarbonate. The aqueous layer is re-extracted with EtOAc (2×). The organic phase is washed with brine, dried with MgSO4, filtered and concentrated under reduced pressure to obtain 63b which dried under high vacuum for 16 h (2.95 g, quantative yield).

References:

US2010/261714,2010,A1 Location in patent:Page/Page column 89

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