ChemicalBook CAS DataBase List 3'-AMINO-4'-FLUOROACETANILIDE

3'-AMINO-4'-FLUOROACETANILIDE synthesis

2synthesis methods

Product Name:3'-AMINO-4'-FLUOROACETANILIDE
CAS Number:113596-04-6
Molecular formula:C8H9FN2O
Molecular Weight:168.17

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Yield:-

Reaction Conditions:

with hydrogenchloride;iron in ethanol;water at 79.84 - 89.84; for 4 h;

Steps:

A3
100 g 4-fluoro-3nitroanilin are added to a stirred mass of 80 g methanol and heated to 333 K. 0.1 ml sulfuric acid and 90 ml of acetic anhydride are added during 15 minutes. Heating and boiling are continued for 15 minutes. Then the reaction mixture is cooled slowly to 273 K with stirring. At the final temperature stirring is continued for 30 minutes, then the suspension is filtered off, washed with cold methanol, dryed in the vacuum dryer getting 114 g acetyl derivative which is worked up further. The acetyl derivative is solved in 520 ml ethanol and continuously added to 130 g iron in 35 ml concentrated hydrochloric acid and 220 ml water at 363K during 1 hour. The temperature drops to 353 K. The reaction mixture is stirred for further 3 hours. The hot mass is separated through filtration the residue washed with 100 ml ethanol. The filtrate and wash solution are cooled to 380 K with mixing, when cristallization of the product takes place. The product is separated by filtration, washed with cold ethanol and dryed in a vacuum dryer.

References:

CIBA SPECIALTY CHEMICALS HOLDING INC. WO2005/97051, 2005, A2 Location in patent:Page/Page column 36