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ChemicalBook CAS DataBase List 2-Amino-3,5-dichloropyridine
4214-74-8

2-Amino-3,5-dichloropyridine synthesis

8synthesis methods
2-Amino-5-chloropyridine

1072-98-6

2-Amino-3,5-dichloropyridine

4214-74-8

General procedure for the synthesis of 2-amino-3,5-dichloropyridine from 2-amino-5-chloropyridine: 5500 mL of a solvent mixture of DMF and methanol with a volume ratio of 2.5:1 was added to a 10L three-necked round-bottomed flask, a thermometer was mounted and configured with condensation reflux device, and a magnetic stirrer was started. 2560.8 g of 2-amino-5-chloropyridine and 6118.4 g of N-chlorosuccinimide were added sequentially, and the reaction mixture was stirred at 45 °C for 2.5 hours. The reaction progress was monitored by TLC and GC until the reaction was complete. After completion of the reaction, the solvent was removed by distillation to obtain the crude product, which was purified by recrystallization with ethanol to afford the target compound 2-amino-3,5-dichloropyridine. The product was dried in 70.5% yield and 98.20% purity (GC analysis).

-

Yield:4214-74-8 70.5%

Reaction Conditions:

with N-chloro-succinimide in methanol;N,N-dimethyl-formamide at 45; for 2.5 h;Temperature;Solvent;

Steps:

3

To a 10 L round bottom three-necked flask was added 5500 ml of a 2.5: 1 mixture of DMF and methanol in a volume ratio of 2.500 ml, inserted into a thermometer and equipped with a condensing reflux device, the magnetic stirrer was started and 2560.8 g of 2-amino- Pyridine, N-chlorosuccinimide 6118.4 g, and the reaction was stirred at 45 ° C for 2.5 hours.TLC and GC were determined to complete the reaction.The crude product was distilled off to give the crude product and recrystallized from ethanol to give pure product 2-amino-3,5-dichloropyridine. After drying, the yield was 70.5% and the purity was 98.20% (GC).

References:

CN104016908,2016,B Location in patent:Paragraph 0027; 0028

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