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ChemicalBook CAS DataBase List Domperidone Impurity 13

Domperidone Impurity 13 synthesis

3synthesis methods
-

Yield:87120-77-2 77%

Reaction Conditions:

palladium-carbon in methanol;

Steps:

7.2 7.2

7.2 4-(2-Nitro-phenylamino)-piperidine-1-carboxylic acid ethyl ester (from step 1 above) was dissolved in methanol then hydrogenated over 10% Pd/C (balloon pressure). The hydrogenation was run until the yellow color turned colorless. It was filtered through a celite pad, and the filtrated evaporated to a reddish brown residue. The residue was triturated with 1% ethyl acetate in hexanes and the solid collected by filtration to give 4-(2-amino-phenylamino)-piperidine-1-carboxylic acid ethyl ester (2.02 g; 77%, 2 steps). 1H NMR (CDCl3) δ1.27 (t, 3H, J=7.2), 1.4 (m, 2H), 2.05 (m, 2H), 3.0 (m, 2H), 3.4 (m, 4H), 4.1 (m, 4H), 6.7 (m, 4H)

References:

US2003/171360,2003,A1

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