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ChemicalBook CAS DataBase List 5-Amino-2,3-dichloropyridine
98121-41-6

5-Amino-2,3-dichloropyridine synthesis

6synthesis methods
2,3-DICHLORO-5-NITROPYRIDINE

22353-40-8

Iron

7439-89-6

5-Amino-2,3-dichloropyridine

98121-41-6

Example 10 Synthesis of 5-amino-2,3-dichloropyridine: 77.2 g (0.4 mol) of 2,3-dichloro-5-nitropyridine was dissolved in 135 mL of glacial acetic acid and 800 mL of water was slowly added under stirring conditions. Subsequently, 111.7 g (2 mol) of iron powder was added in batches, and the reaction temperature was controlled not to exceed 50 °C. After completion of the reaction, the mixture was filtered and the filtrate was extracted using ethyl acetate. The extracted organic phase was washed with water to neutral and subsequently dried with anhydrous magnesium sulfate and concentrated by rotary evaporator. The final product was purified by recrystallization from toluene to obtain 85% yield with a melting point of 107 °C.

-

Yield: 85%

Reaction Conditions:

with magnesium sulfate in water;acetic acid;ethyl acetate

Steps:

10 3-amino-5,6-dichloropyridine
EXAMPLE 10 3-amino-5,6-dichloropyridine 77.2 g (0.4 mol) of 2,3-dichloro-5-nitropyridine were dissolved in 135 ml of glacial acetic acid, and 800 ml of water were added with stirring. 111.7 g (2 mol) of iron powder were introduced in portions into the mixture (temperature≤50° C.). After completion of the reaction, the mixture is filtered under suction and the product extracted using ethyl acetate. The organic phase was washed with water until neutral, dried using MgSO4 and concentrated by evaporation. The product was recrystallized from toluene. Yield 85% Melting point 107° C.

References:

Hoechst Aktiengesellschaft US4756739, 1988, A

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