ChemicalBook CAS DataBase List 2,4-Difluorobenzylamine

2,4-Difluorobenzylamine synthesis

8synthesis methods

Product Name:2,4-Difluorobenzylamine
CAS Number:72235-52-0
Molecular formula:C7H7F2N
Molecular Weight:143.13

3939-09-1 Synthesis

3939-09-1
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$10.00/5g

72235-52-0
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$12.00/5g

Yield:72235-52-0 90%

Reaction Conditions:

with ammonium hydroxide;hydrogen in water;isopropyl alcohol at 60 - 80; under 7500.75 Torr;Temperature;Reagent/catalyst;

Steps:

16; 22 Example 16: Preparation of 2,4-difluorobenzylamine.

Raney Nickel (9.1 gm), 2-propanol (490 gm) and 25% aqueous ammonia (195 gm) were charged into a reactor. The reactor was flushed once with nitrogen and then with hydrogen. The reaction mixture was heated to 60-80°C. Hydrogen was charged in reactor at 60-80°C continuously to 10 kg/cm². A solution of 2,4-difluorobenzonitrile (18% in 2-propanol) was charged in the reactor using a HPLC pump at a rate of 0.5-2ml/min in 12-14 hours. After completion of the reaction, the reaction mass was cooled to 20-25 °C and residual pressure was released. Reaction mass was filtered, washed with 2-propanol (200 gm). The filtrate was concentrated through recovery of ammonia, azeotropic removal of water with 2-propanol. The bottom mass was then purified by distillation under reduced pressure.Yield (%): 90%; Purity (by GC): 99.3%

References:

WO2020/152711,2020,A1 Location in patent:Page/Page column 18; 20-21

72482-64-5 Synthesis