2,4,6-TRIFLUOROBENZYL AMINE synthesis

5synthesis methods

Product Name:2,4,6-TRIFLUOROBENZYL AMINE
CAS Number:214759-21-4
Molecular formula:C7H6F3N
Molecular Weight:161.12

Put into 50 gram 2 into 1000ml autoclave, 4,6- trifluorobenzonitriles, 2.5 grams of raney-ni, 75 gram 25% of ammonia, 500 grams of methanol, control temperature to be 90 DEG C, and mixing speed is 350r/min, are passed through hydrogen hydrogenation, hydrogenation pressure 1mpa, logical hydrogen time 8 Hour reaction terminates, filtering catalyst raney-ni, the methanol in distillation gained filtrate, and distillation terminates addition dichloromethane extraction Take, extract elder generation normal pressure concentrated solvent, then vacuum distillation product, obtain 43.6 grams of product, 2,4,6- trifluoromethyl benzonitrile amine contents 99%, yield is calculated as 85% with 2,4,6- trifluorobenzonitriles.

96606-37-0 Synthesis

96606-37-0
237 suppliers
$6.00/1g

214759-21-4
215 suppliers
$9.00/250mg

Yield:214759-21-4 94%

Reaction Conditions:

with ammonia;hydrogen in isopropyl alcohol at 65 - 75; under 7500.75 Torr;Reagent/catalyst;Temperature;

Steps:

12 Example 12: Preparation of 2,4,6-trifluorobenzylamine
Raney Nickel (8 gm) and 2-propanol (550 gm) were charged into a reactor. The reactor was flushed once with nitrogen and then with hydrogen. The reaction mixture was heated to 65- 75°C. Hydrogen was charged in reactor at 65-75°C continuously to 10 kg/cm². Anhydrous ammonia was charged in the reactor at 65-75°C. A solution of 2,4,6-trifluorobenzonitrile (15% in 2-propanol) was charged in the reactor using a HPLC pump at a rate of 0.5-2ml/min in 10-12 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 and purified by distillation under reduced pressure Yield (%): 94%; Purity (by GC): 97%

References:

SRF LIMITED;SINGH, Amardeep;SINGH, Bhupender;SINGH, Ram;KUMAR, Rajender;CHAUDHARY, Ajay Kumar;KUMAR, Kapil;JAIN, Anurag WO2020/152711, 2020, A1 Location in patent:Page/Page column 16-17

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31881-89-7 Synthesis