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ChemicalBook CAS DataBase List 4-Fluorobenzylamine
140-75-0

4-Fluorobenzylamine synthesis

13synthesis methods
In a 100ml reaction flask, add 25.5g (0.1mol) of N-(4-fluorobenzyl)phthalimide and 25ml of absolute ethanol, then add 6.3g (0.1mol) of 80% hydrazine hydrate solution, and heat Reflux 0.5g. Excessive hydrochloric acid was added to decompose the precipitated white precipitate, after cooling, an appropriate amount of water was added to stir, and suction filtered. The filtrate was neutralized with NaOH solution, extracted with ether, and the ether extract was dried, evaporated to remove ether, distilled under reduced pressure, and collected fractions at 44-46°C (67kPa) to obtain 7.1 g of 4-fluorobenzylamine, with a yield of 56.5%.
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Yield:140-75-0 91%

Reaction Conditions:

with p-tolyl phenylacetate in dichloromethane at 46; for 5 h;Temperature;

Steps:

1 A method for the synthesis of fluoxylated amines from astroxazole intermediates, comprising the steps of:

In the installation of a stirrer,In the reaction vessel of the reflux condenser,A solution of 0.33 mol of N- (4-fluorobenzyl) phthalimide, 180 ml of a 25% methylene chloride solution,Mass fraction37%Of 0.39 mol of p-cresyl ester of phenylacetic acid,Control the stirring speed at 170rpm, raise the temperature of the solution to 46 , reflux reaction 5h;B, add 380ml of 28% potassium bisulfite solution, reduce the temperature of the solution to 15 ° C, add the mass fraction of 40% sodium nitrate solution 280ml, control the stirring speed at 290rpm, pumping, the filtrate by adding the mass fraction for52% of 2,6-dichloro-4-nitrophenol solution 300ml, with the mass fraction of 59% isopropanol solution extracted 8 times, combined to mentionTake the liquid, the mass fraction of 35% potassium bromide solution washing, anhydrous potassium carbonate dehydrating agent dehydration, filtration, 0.83kPa vacuum distillation,The fractions of 60-67 ° C were collected and recrystallized from a 76% acetonitrile solution to give a solution of p-fluorobenzylamine 37.3g 91%

References:

CN106008229,2016,A Location in patent:Paragraph 0024; 0025; 0026; 0027

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