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947255-03-0

3-Fluoro-N*1*-methyl-benzene-1,2-diamine synthesis

2synthesis methods
(3-Fluoro-2-nitro-phenyl)-methyl-amine

947255-02-9
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3-Fluoro-N*1*-methyl-benzene-1,2-diamine

947255-03-0
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Yield:947255-03-0 98%

Reaction Conditions:

with ammonia hydrochloride;zinc in methanol at 50; for 3 h;

Steps:

25.2 (Step 2) 3-Fluoro-N 1-methylbenzene-1,2-diamine

3-Fluoro-N-methyl-2-nitroaniline (0.27g, 1.6mmol) was dissolved in anhydrous methanol (4.5mL), zinc powder (1g, 16mmol) and ammonium chloride (0.43g, 8mmol) were added , heated to 50 , stirred for 3h. The reaction solution was suction filtered, the filter cake was rinsed twice with absolute ethanol (2 mL each time), the filtrates were combined, concentrated under reduced pressure, water (20 mL) was added to the concentrate, and the dichloromethane was extracted 3 times (10 mL each time) , the organic layers were combined, washed once with water and saturated brine, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain the title compound (0.22 g, 98%).

References:

WO2022/156351,2022,A1 Location in patent:Page/Page column 32-33