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2-Pyridinecarboxylicacid,5-chloro-,hydrazide(9CI) synthesis

2synthesis methods
-

Yield:145835-01-4 65%

Reaction Conditions:

with hydrazine hydrate in 1,4-dioxane;water at 100; for 3 h;

Steps:

8.2 Step 2.5-chloropyridine-2-carbohydrazide

To a solution of methyl 5-chloropyridine-2-carboxylate (1.00 g, 6.85 mmol) in 1,4-dioxane (15 mL), was added a solution of hydrazine hydrate (0.60 mL, 80% in H2O). The resulting mixture was stirred for 3 h at 100 °C. Then the reaction mixture was cooled to room temperature and concentrated under vacuum. The residue was purified by silica gel chromatography (eluting with 0:100 to 20:80 ethyl acetate/petroleum ether) to afford 5- chloropyridine-2-carbohydrazide (650 mg, 65%). LCMS (ES, m/z) 172, 174 [M+H]+

References:

WO2020/23802,2020,A1 Location in patent:Paragraph 0601; 0602; 0604