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ChemicalBook CAS DataBase List methyl 2-amino-5-iodo-4-(trifluoromethyl)benzoate

methyl 2-amino-5-iodo-4-(trifluoromethyl)benzoate synthesis

3synthesis methods
61500-87-6 Synthesis
2-AMINO-4-TRIFLUOROMETHYL-BENZOIC ACID METHYL ESTER

61500-87-6
119 suppliers
$19.00/1g

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Yield:872624-52-7 99%

Reaction Conditions:

with iodine;silver sulfate in ethanol at 20; for 2 h;Product distribution / selectivity;

Steps:

3.3

Step 3; Preparation of methyl 2-amino-5-iodo-4-trifluoromethylbenzoate; Add a solution of methyl 2-amino-4-trifluoromethylbenzoate (178 g, 812 mmol) inethanol (3.3 L) to a suspension of iodine (206.1 g, 812 mmol) and silver(II) sulfate (253g, 812 mmol) in ethanol (5 L) at room temperature under an atmosphere of nitrogen andstir for 2 h. Filter the suspension through a pad of a Celite, wash the pad withadditional ethanol (2 L) and remove the solvents from the combined filtrates underreduced pressure at 40 °C. Dissolve the residue in ethyl acetate (7.5 L) and wash withsaturated sodium bicarbonate solution (3 x 1.5 L), water (3 x 1.5 L) and brine (2 L). Drythe organic phase over anhydrous magnesium sulfate, filter and remove the solvent underreduced pressure to give the title compound as a pale brown crystalline solid (276.0 g,99%).

References:

WO2006/2342,2006,A1 Location in patent:Page/Page column 56