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ChemicalBook CAS DataBase List 5-Bromo-N-cyclopropylpyridine-2-carboxamide
638219-77-9

5-Bromo-N-cyclopropylpyridine-2-carboxamide synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

in dichloromethane at 18 - 25; for 2 h;

Steps:

25.1 Step 1: 5-Bromo-pyridine-2-carboxylic acid cyclopropylamide

To a solution of 5-bromo-pyridine-2-carboxylic acid methyl ester [(L.] [OEQ.)] (see Synth. Commun., [1997,] [27,] 515) in THF : MeOH (2: 1; 0.2M) was added aqueous LiOH (1M ; 3. [0EQ.).] The mixture was stirred for 12h, concentrated and dried under vacuum. The residue was diluted in CH2CI2 (0.2M), oxalyl chloride [(8.] [OEQ.)] was added and the mixture was stirred for 3h, concentrated, dried under vacuum and diluted in [CH2C12] (0.2M). Cyclopropylamine [(LOEQ.)] was added and the mixture was stirred for 2h, poured in saturated aqueous [NAHC03] and extracted with EtOAc (2x). The combined organic extracts were washed with brine, dried over [NA2S04,] filtered and concentrated. Flash chromatography (CH2Cl2 : EtOAc; 9: 1) afforded the title compound as a yellow solid.

References:

WO2004/814,2003,A1 Location in patent:Page 69

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