Methyl 3,4-DiaMino-5-chloro-2-Methoxybenzoate synthesis

Yield:-

Reaction Conditions:

with iron;ammonium chloride in ethanol;water; for 3 h;Heating / reflux;

Steps:

1.2 Process 2

A suspension of compound 2 (11.9 g) obtained by the process 1, ammonium chloride (1.22 g, 22.8 mmol) and iron (10.2 g, 183 mmol) in ethanol (450 ml) - water (90 ml) was refluxed for 3 hours. The reaction mixture was filtered through Celite and the remained residue was washed with chloroform - methanol (1:1 v/v, 500 ml). After the filtrate was concentrated under reduced pressure, water (100 ml) was added to the residue and the whole was extracted with ethyl acetate. The organic layer was washed with brine (100 ml) and dried over sodium sulfate. Removal of solvent under reduced pressure gave crude compound 3 (11.6 g) as a dark brown oil

References:

EP1375486,2004,A1 Location in patent:Page 43